JP4922286B2 - Ion implantation system, fluorine chemical supply source, and xenon difluoride supply method - Google Patents

Description

[0001] In this specification, Paul J. et al. Marganski, James I. et al. Dietz and Joseph D.M. US Provisional Patent Application No. 60 / 662,515 filed Mar. 16, 2005 and PAUL J. J., entitled “SYSTEM FOR DELIVERY OF REAGENTS FROM SOLID SOURCES THEREOF” in the name of Sweeney. MARGANSKI and JOSEPH D.M. The priority benefit of US Provisional Patent Application No. 60 / 662,396, filed March 16, 2005, is claimed under the title of SWEENEY under the title “HIGH CONDUCTANCE VALFOR FOR USE IN DELIVERY OF LOW PRESSURE FLUIDS”.

[0002] The present invention relates generally to raw material reagent packaging and substance delivery systems. In a specific embodiment, the present invention relates to the delivery of reagents from solid sources, the corresponding containers for storage and distribution of source reagents, and the delivery of low pressure fluids such as gases or vapors used in the manufacture of semiconductor devices. It relates to highly conductive valves that can be used, and to systems and methods using such valves.

[0003] Chemical reagents are used in various forms. In some cases, chemical reagents are used in vapor form and are obtained from raw materials that are initially solid, for example, at ambient temperature and atmospheric pressure conditions. In such a situation, the solid raw material can be volatilized to form the desired reagent vapor.

[0004] Examples of solid raw materials include decaborane and octadecaborane, which are used as raw materials for boron doping in the manufacture of semiconductors.

[0005] In making a gaseous reagent using a solid source material, the solid material is heated and phased into the gas phase, for example, by sublimation or by causing a continuous solid-liquid-gas transition. Metastasis can be induced.

[0006] Unfortunately, conventional methods of heating solid feeds for such steam generation have many drawbacks.

[0007] Typically, it is difficult to heat a solid source material so that the solid mass of source material is maintained at a desired uniform temperature. This problem is particularly acute with sublimable solids, where non-uniform temperatures can cause vapors to erupt and be released from the solid. This outbreak triggered a pressure perturbation in the reagent delivery system that results in less than ideal evaporation and mass transfer. For these reasons, improving the temperature uniformity of the heated solid has become a fundamental challenge in using solid source materials. Another adverse effect of temperature non-uniformity is the problem of condensation of steam at undesirable locations in the process system, such as transport lines and valves.

[0008] Another problem in using a solid raw material is that a low-density solid has poor thermal conductivity. In many cases, the solid source material is supplied in particles, granules, powders, or other discontinuous forms. In such a discontinuous form, the surface area to volume ratio of the material can be extremely high, and the solid conduction of heat in the particles may be suitable to cause intraparticle heat transfer to occur. The inter-particle gap is a factor in providing limited thermal resistance within the total volume of the particles. Therefore, the bulk density of solids affects conductive heat transfer.

[0009] Another problem that arises when using solid source materials is level sensing of the source material in the supply container. Level sensing is desirable for process monitoring and control of raw material vaporization and vapor delivery from the supply vessel. Since the supply container may be placed in a high temperature environment or may include a heating component to facilitate heat transfer from the container wall to the solid source material contained in the container, the container may be equipped with a level sensor. It can be constrained by the available space or volume limitations that do not allow installation packages. Even if that is not the case, the level sensitive instrumentation package may have an associated temperature limit that is incompatible with the temperature that occurs upon heating the container and the solids therein.

[0010] Another related problem of using solid source materials is the problem of cleaning and recycling the supply container. When the solid matter in the container is evaporated, the solid matter is deposited on the inner wall of the container. Therefore, it is desirable to remove the solid matter from the wall surface after the evaporation operation is completed. The removal of such solids for container reuse can be extremely time consuming, labor intensive, and expensive. Furthermore, the cleaning process itself can introduce further risks, such as toxicity, ignitability, etc., associated with the cleaning agent that must be used.

[0011] For these reasons, the art includes (i) minimizing the adverse effects of temperature heterogeneity on heated material and heat transfer resistance due to voids in the heated solid, and (ii) evaporation Solid source material that is adapted to monitor the level or amount of solids in the supply container as the work is performed, and (iii) facilitates refurbishment and reuse of the supply container after the evaporation operation is complete We continue to look for solutions that make it easier to use.

[0012] As a related consideration in low pressure gas and vapor delivery, the pressure drop that occurs along the fluid flow path in the fluid storage and delivery system components can be a major problem.

[0013] For example, in the manufacture of semiconductor devices, low pressure fluid reagents are typically used for applications such as ion implantation, chemical vapor deposition, etching, and cleaning operations.

[0014] US Pat. No. 5,518,528, which illustrates a low pressure fluid storage and delivery system for such applications, discloses a fluid storage and distribution system based on physical adsorption, in which gas Is stored at a low pressure, for example, at a sub-atmospheric pressure level of less than about 700 torr.

[0015] Other examples include fluid storage and distribution systems described in US Pat. No. 6,089,027, US Pat. No. 6,101,816, and US Pat. No. 6,343,476. Wherein the fluid is disposed in the interior volume and contained in a container having a fluid pressure regulator that operates to discharge through a distribution assembly to a fluid circuit coupled to the semiconductor manufacturing facility. In such systems, fluid can be distributed for use at subatmospheric pressure levels by appropriate selection of the fluid pressure regulator set point pressure.

[0016] Due to the limited pressure driving forces involved in these applications, the flow of low pressure fluid reagent is constrained by system components that have excessive pressure drop characteristics. In this situation, not only the downstream fluid consumption process, but also the products made using the dispensed fluid can have a significant adverse effect.

[0017] Further, when dispensing fluid from a container containing a physical adsorption medium in which the fluid is stored, if there is an excessive pressure drop in a component associated with the fluid supply container, the fluid in the container Even if you want to use it enough, it will be severely restricted. This is because when the fluid is exhausted, the fluid pressure drops to the final level and the fluid distribution becomes unavailable. Therefore, the amount remaining in the container is an "end" that is not usable.

[0018] For example, in certain containers of the type disclosed in the aforementioned US Pat. No. 5,518,528, a gas such as arsine can be stored in the adsorbent. In subsequent use, such gases are desorbed and dispensed, dropping to a pressure of 10-20 torr, after which the system is unable to dispense the gas at a sufficiently high flow rate. If it was possible to reduce the pressure drop in the system components used for dispensing, the dispensing could continue to drop to even lower pressures. As a specific example, if it was possible to perform a continuous dispensing operation down to a pressure of 2 torr, the resulting increase in fluid utilization from the container could be significant, for example about 10%. is there.

[0019] For this reason, low pressure fluids in various applications, such as those exemplified above, in the art to minimize the adverse effects of pressure drops in fluid distribution system components and fluid circuits. We continue to look for solutions that make it easier to send.

[0020] The present invention relates to a system for delivery of reagents from a solid source, packaging of source reagents, material storage and distribution system including containers for storage and distribution of source reagents, and low pressure fluids, eg, semiconductors It relates to highly conductive valves that can be used to deliver gases or vapors used in the manufacture of devices, as well as systems and methods using such valves.

[0021] In one aspect, the present invention is a structure configured to hold a solid source material in order to heat the solid source material and generate vapor from the solid source material by evaporation. A structure containing in part the solid source material, a heat source configured to heat the solid source material for such evaporation, and a vapor distribution assembly configured to release steam from the system. It relates to a system for delivering a reagent from its solid source.

[0022] In another aspect, the present invention holds a solid source material encapsulated by at least a part of a holding structure, and heats the solid source material to generate vapor from the solid source material by evaporation thereof. And a method for delivery of reagents from a solid source comprising receiving such vapors.

[0023] The present invention, in other aspects, relates to a valve having an excellent valve flow coefficient that can be used for delivery of low pressure fluid, and a system and method using such a valve.

[0024] In one aspect, the present invention provides a valve main body that defines a valve chamber therein, an inlet passage that communicates with the valve chamber and allows fluid to flow into the valve main body, and communicates with the valve chamber to allow fluid to flow out of the valve main body. And an actuator for allowing movement of the valve element between a fully open position and a fully closed position within the valve chamber, the inlet passage and the outlet passage when the valve element is in the open position. In conjunction with the valve chamber, it relates to a highly conductive valve that allows fluid to flow through the valve body, the inlet passage and the outlet passage being substantially perpendicular to each other.

[0025] Another aspect of the invention relates to a fluid delivery system comprising a valve of the invention coupled to a fluid container.

[0026] Yet another aspect of the present invention relates to a system for manufacturing a semiconductor comprising a valve of the present invention coupled to a semiconductor manufacturing facility.

[0027] Yet another aspect of the present invention is to allow the valve to have a flow controlling relationship with the fluid and to distribute the fluid to the fluid consumption process at the rate required by the process. Selectively opening, the method of using the valve of the present invention.

[0028] Still other aspects of the invention include placing a reagent in a container and selectively opening a valve to dispense the reagent from the container to a fluid consumption process at a rate required by such process. To a method of using the fluid delivery system of the present invention.

[0029] Other aspects, features and embodiments of the invention will become more fully apparent when the following disclosure and appended claims are read.

[0059] The present invention relates to systems and processes for delivering reagents from solid sources.

[0060] In one specific embodiment, the present invention relates to a solid raw material for semiconductor production, including a solid raw material such as decaborane, octadecaborane, indium chloride, which can be used by sublimation because of its low melting point and considerable vapor pressure. Beneficially used to evaporate material.

[0061] In many cases, in order to generate low pressure vapor from a solid source material, the delivery rate of the evaporated reagent is sufficient to meet the requirements of downstream processing systems that use such evaporated reagent. There is a need for highly conductive fluid circuits and components. In this regard, a particularly useful high conductivity flow control valve is shown in FIGS.

[0062] Referring now to the drawings, FIG. 1 is a schematic front view showing a partial cross section of a system 10 for delivering reagents from a solid source material, according to one embodiment of the present invention.

[0063] The reagent delivery system 10 includes a container 12 having a floor 32, a side wall 34, and an upper wall 36 that define an enclosed internal volume 14 into which a mass 30 of solid source material enters a lower portion of the container. .

[0064] The container 12 in the internal volume 14 includes a porous plate member 16 having a series of channel openings therein extending from the bottom surface of the plate member to the top surface thereof. The plate member 16 further includes interconnected holes 20 but not in communication with the flow path openings 18. The plate member 16 is connected to the shaft 22 in the central region and, in one embodiment, is formed as a telescopic tubular assembly.

[0065] In one embodiment of the system shown in FIG. 1, the telescopic shaft 22 is surrounded by a helically extending bias spring 24. The shaft 22 and the spring 24 are fixed to the upper wall 36 of the container 12 at the upper end thereof, and are fixed to the central region of the plate member 16 at the lower end thereof. With this arrangement, the spring 24 functions to apply a compressive force to the upper surface of the plate member 16 and push the plate member downward, thereby maintaining contact with the upper surface of the solid material mass 30 and compressing the plate member 16. Support with power.

[0066] The solid source material mass is suitably sized as a suitably sized particle that maximizes the surface area to volume fraction of the material, for example, in a suitable form such as a granulate, powder, or other discontinuous form. be able to. In other embodiments, the solid source material mass is formed in a single monolithic block form, for example, by solidifying the source material liquid after heating for a volume of the material that was initially solid. Can be. The monolithic block of source material is not high in surface area to volume ratio, but nevertheless has no voids that can impede heat transfer throughout the bulk volume of the corresponding particulate mass of solid source material. The solid source material can be heated by microwave heating the solid source material or by applying heating energy by other methods.

[0067] The plate member 16 of one embodiment of the system of FIG. 1 is heated and pressed against the top surface of the source material 30, the hot plate member evaporates the source material in contact with this member, and then The resulting vapor flows through the plate member flow passage openings 18 into the upper internal volume of the container.

[0068] Heating of the plate member 16 and the associated solid source material can be performed by any suitable method. Various types of heat transfer configurations can be used to provide such heating, with various suitable heat transfer, such as heat transfer fluid, which may be gas or liquid, as appropriate, for example. Use media. In one embodiment of the invention, the shaft 22 is hollow and the hollow interior passage is in communication with a sump and pump assembly attached to the top wall 36 of the container. The liquid in the sump and pump assembly 76 is heated by a passage in line 86 from the sump sump to the heat exchanger 82 and the liquid is heated to the appropriate temperature to evaporate the solid source material and heat it. The resulting liquid is returned from the heat exchanger to the sump and sump of the pump assembly 76. The liquid is then pumped into a hollow passage inside the shaft 22 by a pump in the sump and pump assembly, from which hot liquid flows into the internal holes 20 of the plate member and circulates through the holes as the pump is activated. Then, it is returned to the liquid reservoir in the assembly 76. For such recirculation of heat transfer fluid back to the sump, the interior of the shaft 22 is provided with an appropriately sized recirculation path so that the pressure drop and drive force provided by the sump and the pump in the pump assembly 76 is reduced. At reflux.

[0069] In this way, the continuous liquid flow through the plate member 16 causes the temperature of the plate member to evaporate the solid source material near the plate member when the plate member is pushed downward by the spring of the bias spring 24. To maintain a sufficient temperature.

[0070] Next, the evaporated solid source material flows through the plate member channel opening, and moves upward in the direction indicated by the arrow M, and is disposed on the upper surface of the upper wall 36 through the upper wall 36. It flows to a filter 50 that is connected to a discharge pipe 52 that is connected to a conductive valve 54. The filter 50 is a feature that is optionally included in the solid source material container and may not be present if it is not necessary to remove particles in the vapor flow path or otherwise restrict the flow rate. High conductivity valve 54 includes a valve body 56 to which a discharge fitting 60 is coupled. Although the valve comprises a hand actuator 58 in the illustrated embodiment, the valve 54 may be an automatic actuator or other so as to selectively open the valve 54 for distribution of vapor derived from the solid source material in the container. It can be configured in various forms with the controller.

[0071] A particularly suitable high conductivity flow valve useful in practicing the invention extensively is shown in FIGS. 25-29, as described in more detail below.

[0072] In the illustrated configuration, as the solid source material sublimes and the lump 30 gradually decreases, the biasing operation of the spring 24 maintains the contact between the plate member and the source material. Solid source material level sensing provides an output indicating the level of the plate member in contact with the bulk volume top surface of the solid source material, thereby generating source material vapor, so that the solid source remaining in the container It can be done in a configuration that uses electrical contact (s), or magnetic, optical, or other sensors that provide output reflecting the amount of material.

[0073] In another configuration of FIG. 1 in which the plate member is heated, the source material changes to the gas phase and is consumed and the plate member is pushed downward, the sump and pump assembly 76 is heated and the sump and pump assembly is heated. The main oil reservoir 78 of the hydraulic oil pumped into the hollow passage of the telescopic shaft 22 can be coupled by 76. Then, the heated hydraulic oil flows into the hole 20 of the plate member 16 and is pressurized at the same time. The hydraulic pressure is applied to the plate member and pushed downward. At this time, the telescopic shaft 22 extends downward. In this way, contact between the heated plate member 16 and the upper surface of the solid source material is maintained.

[0074] Various alternative or additional force mechanisms may be used in certain embodiments of the present invention to maintain contact between the plate member 16 and the top surface of the solid source material. For example, a movement transition can be imparted to the plate member by a change in the momentum of the heat transfer fluid that is in contact with the plate member and flows away therefrom. Further, the downward pushing force is present due to the weight of the plate member 16, and therefore the plate member weight is selected to help maintain strong contact with the solid source material mass in the container. can do. Further, by adding weight to the plate member, it is possible to increase the force for maintaining the contact between the plate member and the solid source material. Accelerating the mass of a plate by applying an acceleration field (gravity field, electric field, etc.) is another force mechanism that can be used.

[0075] Also, in some applications of the embodiment shown in FIG. 1, the plate member 16 may be used as a mere member that applies pressure to the mass of solid source material without directly heating it, and the container may be heated. However, it may be convenient to use. For example, if the plate member 16 and the telescopic shaft 22 are made of a highly conductive material, such as aluminum, there is sufficient heat conduction from the container wall to transfer heat to the plate member from which heat is transferred to the solid source material surface. Can be moved. Relative heating of the vessel wall and heating of the plate member should be performed so that the plate member temperature does not rise above the vessel wall temperature as necessary to avoid condensation of vapor derived from the solid source material.

[0076] Generally, the container is heated externally so as not to condense after the vapor is generated. For this purpose, the container is heated by a heating jacket 38, 40, 42, and a steam space heating jacket that surrounds the outside along the part of the container that the solid source material contacts when the steam is being distributed gradually. 39 can be provided. The configuration of the surrounding heating jackets 38, 40, and 42 allows the level to be indicated by monitoring the air pressure or hydraulic pressure inside the telescopic strut of the shock absorber type configuration, when the fluid is The pressure of the fluid decreases as the strut lengthens as the source material gradually wears. Each heating jacket is shown in schematic form, with no associated electrical wires and power sources, for ease of explanation.

[0077] The upper heating jacket 38 surrounds the side wall 34 of the container 12 and is the boundary of the upper heating zone designated "A". The intermediate heating jacket 40 surrounds the side wall 34 of the container below the zone “A” and is the boundary of the intermediate heating zone “B”. The lower heating jacket 42 surrounds the side wall 34 of the container 12 and is a boundary of the lower heating zone “C”. Each heating jacket can be coupled to a suitable energy supply component, eg, a power source, each one of the jackets being associated with an associated zone of solid source material by conductive heat transfer through the sidewall and into the solid source material. Operated for heating.

In this way, the upper heater 38 operates when the solid source material is in zone “A” and the intermediate heater 40 is in the zone “B” while the solid source material is in zone “B”. Activated when not in “A”, lower heater 42 is activated when the solid source material is in zone “C” but not in either zone “A” or “B”. As a result, when the solid source material in the corresponding zone is heated, as described above, the vapor generated from the solid material passes through the flow path opening 18 in the plate member 16, and passes through the filter 50 and the high conductivity flow rate control. Valve 54 is entered and fluid is dispensed.

[0079] In this way, the object of heating becomes a small section of solid matter. In this way, the target of the heating action is also narrowed down to a specific region of the solid material by pushing the solid material against the stationary porous or perforated plate member, for example, by a mechanical feeding device that is carried up be able to. Alternatively, the solid source material can be placed in a container that independently translates into a heating zone such as a furnace or oven. In these alternative arrangements, only one heating zone is required. However, to avoid vapor condensation and undesired redeposition of solids in the downstream region, it is close to the solids regardless of whether there is one or more heating zones to evaporate the solid source material It will be appreciated that the heating zone must be cooler than the area downstream of the solids.

When distributing the fluid, the vapor from the raw material solids passes through the valve 54 and the discharge fitting 60 and flows into the fluid distribution pipe 62 in which the flow control unit 64 is stored. The flow control unit 64 is a simplified representation of components used in a flow distribution circuit such as, for example, a mass flow controller, temperature and pressure sensors, flow control valves, fluid pressure regulators, flow restriction orifice elements, and the like.

[0081] The dispensed fluid then flows through distribution line 62 and enters processing facility 66, which may include, for example, a semiconductor manufacturing facility or other facility in which the dispensed fluid is utilized. it can. Utilization of fluid in the processing facility 66 may generate waste liquid that is discharged to the waste liquid removal complex 70 in line 68, where the waste liquid is eliminated and made safe or other It is made suitable for discharge into the pipeline 72 in some way.

[0082] The vessel 12 can be changed to shutdown when the solid source material is completely exhausted. The shaft 22 can then be retracted so that the plate member is above the height of the solids inlet 44 on the side wall 34 of the container. Next, the solids inlet is opened, the container is refilled with solid source material, and the container after refilling the inlet 44 is returned to be used for dispensing fluid derived from the solid source material. . As another alternative, the top wall 36 of the container 12 can be formed so that it can be removed from the rest of the container, so that such top cover can be removed and fresh solid source material can be removed from the container's internal volume. Can be refilled. For such purposes, a flange member that can be fitted to the top cover to cooperate with a corresponding flange member at the upper end of the side wall 34, such as removable fasteners such as bolt and nut assemblies or the like. Each flange fixed by a coupling member can be machined to facilitate such removal of the top cover.

[0083] When the operation is stopped after the evaporation operation is completed, the container may be restored by performing appropriate cleaning and regeneration operations on the container, and the operation may be resumed by refilling the container with a new solid source material. it can. To minimize downtime for such temporary cleaning and refilling operations, use disposable liners that are dropped into the container with fresh storage solids after the previous storage solids have evaporated All that is required is that the disposable liner already containing the initial filling of the solid source material is simply removed from the container and discarded. Such a disposable liner is another aspect of the present invention.

[0084] Therefore, the use of the liner facilitates refilling of the container. In many cases, a non-volatile residue can be formed after the solid source material has been heated for an extended period of time. This residue is extremely difficult to remove when present on the inner wall of the container holding the solid source material. Therefore, when a disposable liner or bag is used, the reusability of the solid material container is greatly increased.

[0085] The container is actually provided to the user by the manufacturer or point of sale in a closed state, but when the container is connected to the valve and discharge line, it is returned to the manufacturer for repair You can leave it closed in some other way. Once delivered, the manufacturer can open the container for cleaning. If a liner or bag is used, the manufacturer simply opens the container, removes the bag, discards it, puts it in a new bag with a single solid source material, or puts it in the container empty and then solids Insert a bag filled with source material.

[0086] As another variation, a non-disposable liner can be formed from a material that can be easily cleaned, and therefore a liner bag that is not thrown away is simply placed in a single wash solution, The accumulated solid matter or the like can be solubilized with a cleaning solution or chemically reacted to regenerate and reuse the bag.

[0087] A disposable or some other reusable liner has structural integrity and properties under high temperature evaporation conditions where the solid source material must be exposed to form the desired vapor. For example, a polymer such as polyimide or polysulfone.

[0088] The solid source material container in the system of the present invention may include a level sensor that generates an output indicating the remaining amount of the solid source material in the container. In one embodiment, the level sensor comprises an inert gas source coupled to the container with a fluid circuit that pulses a known volume of inert gas into the container, and the pressure transducer is a solid source material container A corresponding pressure measurement of the pressure in the internal volume of the chamber and a pressure response signal indicative of the amount of solid chemical remaining in the container.

[0089] Separately, the amount of inert gas injected to increase the pressure in the internal volume of the solid raw material container to a predetermined value also indicates how much solid chemical substance remains in the container. Information is obtained. In this case, it is also possible to use a mass flow controller and measure the inert gas into the solid material container.

[0090] In each of these level sensing configurations, the level sensing operation occurs when the container is isolated from the fluid utilization process used in normal operation by the container. For this purpose, the solid material container can be operated to be on-line for a short time during normal dispensing operations to accommodate level sensing tests. In order to be able to perform such tests without interrupting the work of supplying steam to the downstream fluid utilization process, a system with a surge tank or having a hold-up volume can be used when there is no flow. A certain amount of steam can be replenished when performing the level detection test of the solid material container.

[0091] In yet another alternative configuration, when the solid source material is heated to the melting temperature in the vapor distribution operation, the float switch is used to sense the liquid level of the liquefied source material in the supply container, An output indicating the amount of the solid source material (liquefied form) can be obtained.

[0092] In yet another alternative configuration, a flow summing device can be used to sense the remaining amount of solid source material (or liquid material if liquefied) remaining in the container, This operates to sum the flow data coming from the flow regulator used to modulate the flow of steam from the supply vessel.

[0093] In yet another configuration, the solid source container can be processed to house a level sensor that senses the position of the plate member 16, so that it must still be evaporated and distributed within the container. An output indicating the amount of solid source material that must be generated can be generated. In one embodiment, such a level sensor comprises one or more level switches in the wall of the solid source container that engage when the plate member 16 passes the switch. In other embodiments, the level sensor is mounted on a detector that can be mounted, for example, within the cover of a solid source material container and that can output a signal that correlates to the position of the plate member within the interior volume of the container. A laser is provided that can be configured to generate a reflected light beam. With these configurations, the level of the solid source material in the container is monitored and the output, for example, the form of data stored in the central processing unit (CPU), and / or the container content of the solid source material will soon be It can be generated in the form of a visual and / or audible alarm when it is about to run out and needs to be switched to a new container and replaced.

[0094] In another method that can be used to monitor the remaining amount of solid source material in a container, a steam generation system can be constructed and steam derived from the solids can flow through the shaft 22. Then, the strut is brought into communication with the high conductivity flow control valve 56. In this embodiment, there will be no heat transfer fluid in the shaft 22. With this configuration, the internal volume 14 can be monitored by pressure. If there is no leak in the internal volume 14, the pressure in such a volume decreases when solid material is used and the plate member 16 is pushed down. The corresponding pressure signal can then be used to indicate the solids level of the container internal volume at a predetermined time during the steam distribution operation.

[0095] The container containing the solid source material can be heated by suitable means such as microwave heating, infrared heating, other methods of radiant heating, conductive heating, convection heating, electrical resistance heating, and the like. If the method of generating vapor from solid source material is used as a reagent for the manufacture of semiconductor products, when a new solid source container is installed for vapor distribution, the container is already In some cases, it may be convenient to heat the container away from the semiconductor manufacturing facility, such as at temperature. Mounting the container “at a certain temperature” seems to be useful in reducing start-up and transition times in the semiconductor manufacturing plant and maintains a significant percentage of the “uptime” when it is in operation. Is critical to the economic continuity of production facilities.

[0096] FIG. 2 is a schematic front view showing a partial cross section of a system 100 for delivering reagents from a solid source material according to another embodiment of the present invention.

[0097] The system 100 includes a container 102 that defines an enclosure in which a quantity of solid source material 106 is placed as a fluidized bed or a single mass within the container. In this embodiment, the channeled plate member 108 is attached to the lower end of a threaded conveyor screw 128 that engages in a threaded collar 126 attached to the top wall of the container.

In this embodiment, the conveyor screw 128 is originally driven downward by the drive gear 132 of the drive unit 130. The drive unit 130 is reversible with respect to the rotation of the drive gear 132 so that the conveyor screw can be driven in either the vertical upward or vertical downward direction indicated by the double arrow R. During the dispensing operation, the conveyor screw is driven downward to maintain the pressure on the plate member.

[0099] The solid source material 106 is simultaneously heated in a suitable manner (heating means not shown in FIG. 2), so that the vapor exits the container in the direction indicated by arrow P, and filters 112, Flowing through a highly conductive flow control valve 110 and a fluid discharge line 114, within which is a flow control unit 116. From the fluid discharge line 114, steam derived from the solid source material enters the downstream processing facility 118 where it is used.

[00100] In such use, a waste liquid flow may be generated, and such a flow is flowed from the processing equipment 118 to the waste liquid reduction equipment 122 through the pipe line 120 and processed. As a result, the discharge pipe 124 Purified waste liquid is discharged from the system.

[00101] The remaining amount of solid source material in the container 102 during dispensing can be monitored by the simple configuration shown in FIG. 2, where the conveyor screw 128 is engaged with the gear 136 of the monitoring unit 138. In response to the rotation of the gear 136, a control signal is generated by the monitoring unit 138 and passed to the CPU 142 via the signal transmission line 140. The CPU may be of any type as long as it is connected to the monitor 144 and is suitable for outputting the remaining amount information in a graphic and / or text format, for example, as shown in the figure. It can be a programmable computer.

[00102] FIG. 3 is a schematic diagram illustrating a configuration for depositing vapor of a solid source material on a physical adsorption medium in a storage and distribution vessel. In another different aspect discussed in the present invention, a physical adsorption medium and / or solid source material is coated on a high surface area / high thermal conductivity medium such as metal beads to evaporate the solid source material. A large surface area and high thermal conductivity can be obtained. Such a configuration overcomes the disadvantages of powders or monolithic blocks with a low packing density of solid source material.

[00103] In this configuration, the solid source material 182, in order to put enough heat energy Q ₁ to sublimate the solid raw material, is stored in the supply container 180 provided with a heating jacket 184 associated with it. The resulting solid source material vapor flows through line 186 to an inlet 190 of a storage and distribution vessel 194 containing a physical adsorption bed 196 such as activated carbon or molecular sieve. The adsorbent is selected to have an adsorption affinity for the solid source material vapor, and therefore the adsorbent absorbs the solid source material vapor and holds it in an adsorbed state.

[00104] The container 194 includes a valve head 192 that houses the inlet 190, dispensing port 200, and handwheel actuator 198 described above, as shown.

[00105] FIG. 4 is a schematic diagram illustrating the storage and distribution vessel 194 of FIG. 3 in a subsequent distribution mode in which adsorbed feedstock material is desorbed and utilized in a downstream fluid utilization process system.

[00106] As illustrated, the container 194 is placed on the configured heated jacket to the heat input Q ₂ is fed to the vessel that contains the adsorbent which is packed with adsorbent solid source material vapor, However, the heat flux Q ₂ is assumed to be large enough to desorb sorbate vapor from the adsorbent. A valve in the valve head 192 is opened by manually moving the handwheel 198 so that fluid is dispensed from the dispensing port 200 and represents a schematic of the fluid circuit and monitoring and control components. Fluid flows into the conduit 202 containing 204 and enters the fluid utilization facility 206 where the fluid is used. By using in this way, a waste liquid flow that flows to the waste liquid treatment facility 210 is generated in the pipe line 208, processed, and discharged into the pipe line 212 of the last purified waste liquid.

[00107] FIG. 5 is a perspective view of a source reagent article 216 according to another embodiment of the present invention, including a core body 220, coated with a solid source material 216. As shown in FIG. Such articles can be used in place of the adsorbent medium as described with reference to FIGS. 3 and 4, so that articles coated with a plurality of solid source materials can be stored in storage and dispensing containers. And can be selectively heated as it is in the container to release the vapor from the solid source material coating.

[00108] The core body for such purposes may be of any suitable size, shape, and structure. Instead of the rod shape shown in FIG. 5, the core body may be spherical, ring or donut shaped, cubic, spiral, flat ribbon shaped, mesh shaped, needle shaped, conical, or other geometric or non-geometric This can be of a specific shape or form, depending on the heating and release of the vapor from the solid source material coating on the core body.

[00109] FIG. 6 is a schematic diagram of a delivery system 250 that uses a solid source material, according to yet another embodiment of the present invention.

[00110] In the system of FIG. 6, a solid source material supply vessel 256 is configured to supply in a conduit 258 of a solubilization tank 260 with a mechanical agitation function schematically illustrated by an impeller 262. Yes. The solubilization tank 260 is simultaneously supplied from a conduit 266 from a solvent supply container 264 containing a solvent having an effect of easily dissolving the solid source material under the mixing conditions obtained in the solubilization tank 260.

[00111] Solvents can be easily selected based on solubility data for the solid source material of interest and volatility data for such solvents. Thus, the solvent solubilizes the solid source material in the solubilization tank 260, and the resulting solution flows from the tank 260 via line 268 to the filtration or screening unit 270, which causes the solids to flow sequentially in the system. The flow in the direction is hindered. Solids, if present, are recovered and recycled to tank 260 via line 272 for mixing and subsequent resolubilization. Unit 270 separately includes a centrifuge, clarifier, settling tank, or other separation unit so that solids are separated if present and recycled to solubilization tank 260. .

[00112] The resulting solid-free solution flows in line 274 into a storage and distribution vessel 252 that in this embodiment comprises a heating jacket 254. Container 252 is filled with a support material bed, such as adsorbent particles, and / or a non-adsorbent medium in the form of, for example, a ring, flake, disc, cylinder, cube, pyramid, sheet, rod, or other structure. Such a medium can include a material having a high specific heat or thermal conductivity to facilitate subsequent heating operations, as described below.

[00113] When the solution containing the solid source material settles into the internal volume of the container 276 containing the adsorbent or other medium therein, the container 276 is activated by the heating jacket 254, so that the solid source material solution The solvent is heated to a temperature (e.g., in contact with and into the pores of the adsorbent material or other carrier and on the vessel wall), leaving the solid source material in the vessel after evaporation. The evaporated solvent flows from the vessel 276 into the conduit 278 and flows through the chiller / condenser unit 280, where the solvent is condensed into a liquid. The resulting liquefied solvent then flows into the recirculation line, enters the solvent supply vessel 264, and is reused to replenish a fresh solution of solid source material.

[00114] Once all the solvent has evaporated and recycled in the system, the remaining solid source material is left in the vessel. Next, when the container is heated again to evaporate the solid source material in the container, the resulting vapor flows from the container to the conduit 282 and enters the fluid utilization facility 284.

[00115] In order to correspond to the respective heating steps in which the solvent is separated in the first step and the solid source material is evaporated in the second step, valves are appropriately attached to the pipe lines 278 and 282, and the heating step is sequentially performed. In each case, vapors derived from the respective solvents and solids are directed to the appropriate line.

[00116] Utilizing solid source material vapor in the facility 284 may result in waste liquid that requires treatment, and this situation is provided with a waste liquid line 286 that carries the waste liquid to the treatment facility 288 and is purified therefrom. This is dealt with by allowing the final waste liquid to be discharged into the pipe 290.

[00117] FIG. 7 is a diagram of a reagent delivery system 300 using a solid source material 308, according to another embodiment of the present invention.

In the system of FIG. 7, the solid source material storage container 302 stores a bag 336 of solid source material 308. The upper free end of the bag 336 is folded over the upper end of the container 302 and held in place by a cover 304 for the container. Container 302 is surrounded by a selectively operable heating jacket 310 for heating the container and bag within its internal volume 338.

[00119] The cover 304 has a heating unit 318 having an infrared heating lamp 320 attached to the lower side of the cover, and the infrared G is applied to the solid source material bed 308 contained in the bag 336. If a laser is used as a coherent radiation source instead of using infrared, the solid source material can be heated very selectively to generate steam. Regardless of the specific method used to perform the heating, as a result of the heating, the solid source material generates vapor that rises through the upper space 306 in the bag, and the filter 332, the high conductivity flow control valve 330, and It passes through the distribution fitting 360 and enters the discharge flow line 362 containing the flow control unit 364. Thereafter, the distributed solid source material vapor flows into the utilization facility 366, from which waste liquid flows into line 368 and enters the treatment facility, where the treated waste liquid discharged from the system is generated in line 372.

[00120] The container 302 has an inlet 312 on the cover. A vacuum line 314 coupled to the vacuum pump 316 can be connected to the inlet 312 so that the gas can be discharged from the container before being heated to generate vapors of solid source material. Alternatively, the flow can be reversed in line 314 to allow carrier gas or other fluid to flow into the vessel to facilitate the generation of solid source material vapor. Such carrier gas or added fluid can be heated to direct sensible heat into the vessel and help sublimate the solid source material.

[00121] The bag 336 of the system of FIG. 7 can be made of any suitable material, such as a polymer, metal, resin-coated woven fabric. In a preferred embodiment, the bag is formed from a film material that is aluminized or otherwise metallized, so that the infrared rays that have been impinged on the solid source material when the system of FIG. 7 is operating. Reflect. The bag can constitute a disposable or reusable liner, which can be discarded as described above or, for example, solid deposits and other residues can be removed from the bag sheet or film By soaking in a suitable cleaning solution for a time suitable to be removed from the material, cleaning and regeneration operations can be performed.

[00122] As another and optional feature, the solid source material contained in the bag is agitated by means of pulsing argon, nitrogen, or other suitable gas into the space between the bag and the sidewall. Or it can be vibrated to deform the bag so that the solid source material in the bag is mixed so that vapor generation from the solid source material is maximized. For this purpose, the gas supply 342 may be coupled to the reversing pump 340 using a gas supply line 346. As the pump 340 reciprocates, this causes gas to be injected into the conduit 348 between the bag and the sidewall of the container, which is then pumped out of the container. It is drawn from such a space (between the bag and the side wall) and discharged from the pump into the discharge line 350. In this way, the bag is subjected to alternating operations of repetitive compression and suction, whereby the contents of the bag are continuously mixed and the generation of vapor from the solid source material is maximized.

[00123] FIG. 8 is a diagram of a reagent delivery system 400 that uses a solid source material, according to an additional embodiment of the present invention.

[00124] The system of FIG. 8 includes a container 402 containing a solid source material particle bed 404. As one of several variations, a mixing screw 406 coupled to the drive assembly 414 can be disposed in the container. The drive assembly can include, for example, a motor and associated gearing for rotating the mixing screw 406 about the longitudinal axis so that the solid source material in the container can be moved when the container is in operation. Mixing continuously with the heat entering from the heating jacket 448 maximizes steam generation and prevents heat from becoming uneven in the solid particle bed.

[00125] Alternatively or in addition, vertically extending heat transfer fin assembly 408 and / or horizontally extending heat transfer fins in vessel 402 to maximize solid conduction in the solid feed particle bed The assembly 410 can be in place.

[00126] The vapor generated by evaporating the solid source particles in the container 402 is discharged from the container into the pipe line 420 under the momentum of the recirculation pump 422, and the vapor is recirculated by the pump. And is recirculated back to the vessel 402 and a portion of the flow is extracted from the recirculation loop 424 and flows through a conduit 440 that includes a pressure sensor 442, a mass flow regulator 444, and a temperature sensor 446. The semiconductor manufacturing facility 450 arrives.

[00127] The recirculation loop 424 is supplied with a carrier gas supplied from an inert gas supply source 430, from which an inert gas or other carrier gas flows into the conduit 432, such carrier. A regulator 434 is entered for fluid pressure regulation of the gas flow and is expelled into line 436 to enter the recirculation loop.

[00128] After being injected into the recirculation loop 424, the carrier gas flows into the in-line heater 416 and is heated so that the temperature of the solid source material in the vessel is substantially uniform. The carrier gas then flows through the container 402.

[00129] The pump 422 in the recirculation loop 424 forms a pressure head in front of the mass flow regulator 444 with the injection of carrier gas into the recirculation loop so that the mass flow regulator It can operate more effectively than if pure steam is delivered to the facility through a mass flow controller. As the mass flow regulator opens, the pressure in the recirculation loop 424 drops, thereby drawing more carrier gas. This tends to maintain a constant pressure in front of the mass flow regulator.

[00130] The recirculation loop 424 may include a check valve 426 in front of the carrier gas inlet, as shown. The system can control the flow of the source chemical by using a simple orifice instead of the mass flow regulator 444 and controlling the pressure in the recirculation loop 424.

[00131] The system of FIG. 8 operates such that the major portion of the carrier gas / chemical mixture that is expelled from the container into conduit 420 is recirculated back to container 402. This ensures that the carrier gas contains a chemical component, for example, a chemical component that is approximately equal, if not equal, to the equilibrium vapor pressure of decaborane.

[00132] The temperature sensor at the outlet of vessel 402 and the pressure sensor in line 440 are incorporated into a monitoring and control scheme used to modulate the heating of in-line heater 416 and heating jacket 448 to provide a raw solid A predetermined temperature and pressure of the chemical stream can be directed from line 440 to equipment 450.

[00133] FIG. 9 is a schematic perspective view of an annular reagent dispensing container 460 according to another aspect of the present invention, which is capable of internal positioning of a heating jacket 466 on an outer surface along with a heating insert 476.

[00134] The toroidal vessel 460 is toroidal with an internal cavity 464 defined by the annular inner wall 462 of the vessel. The container inlet or vapor discharge passage is not shown in FIG. 9 for simplicity. The container contains a batch of solid source material, and the internal cavity 464 is shaped to receive a correspondingly shaped heating insert 476, which is an insertion unit for electrical resistance heating by insertion of the container 460. Can be provided with a power cord 478 for connecting to the power source.

[00135] Thus, as shown in FIG. 9, the heating insert 476 is inserted upward and into the cavity 464 of the container 460. The container cavity includes a positioning coupler 470 that is mated to cooperate with a complementary shaped positioning element 480 on the top surface of the heated insert. Thus, such complementary mating structures 470, 480 ensure that the heated insert and container are properly positioned before heating by the container insert begins. In one embodiment, the mating structures 470, 480 can be configured to prevent the heated insert from acting unless the positioning element 480 and the positioning coupler engage each other.

[00136] The container 460 may further include an outer heating jacket 466 on the outer surface, whereby the annular wall is most effectively heated to generate steam from the solid source material in the container. .

[00137] FIG. 10 illustrates an embodiment of the present invention comprising a series of horizontal trays 510, 512 in a stacked structure, each tray being coated with or containing a solid source material. 6 is a front view showing a partial cross section of a reagent delivery container 500. FIG.

[00138] Container 500 includes a dispensing valve 504 coupled with a suitable dispensing fitting 506 for connecting the container to a dispensing fluid circuit, as illustrated, having a cylindrical enclosure wall 502. A container within the internal volume includes a stacked array 510, 512 of trays coated with or otherwise containing solid source material. The tray in the illustrated embodiment includes protrusions that mate with protrusions on adjacent trays to form an array of stacked trays. The trays in the stacked arrangement can be formed of suitable constituent materials, but are preferably formed of a highly thermally conductive material such as aluminum, copper, nickel, and the like.

[00139] The container 502 is heated by an electrical heating tape 520 that is continuously wound around the container as shown in the figure and terminates at a free end 522 to heat the tape, thereby Electrical resistance heating wires 526 and 528 extend from the free end 522 and couple to a power source or other electrical energy source for heating. As a result, the container is heated and the tray within effectively transfers heat to the solid source material on or in the tray, generating steam that is distributed from the container. Alternatively, the container 502 can be heated by a molded heating jacket that fits closely with the container and is in intimate contact to transfer heat.

[00140] FIG. 11 is a perspective view showing a partial cross section of a reagent delivery container 552 according to another aspect of the present invention incorporating an internal fluid collection manifold 566 associated with a porous tube 570 and / or a porous ring 568. It is.

[00141] The system 550 of FIG. 11 includes a generally cylindrical container 552 having an upper wall 560, as a cylindrical inner container connected to the upper wall, followed by a porous tube 570 and a porous ring 568. Mounted is a distribution valve 562 that is joined by connecting a tube 564 to a manifold 566. The purpose of the porous tube and ring member is to accept the inflow of vapor from the solid source material after heating. The solid source material 554 is contained in the internal volume of a container 552 that encloses the porous tube and ring member therein.

[00142] In this embodiment, thermocouples 590 are placed in a solid source material bed and lined up along the length to monitor the temperature of the solid source material bed along the entire height. Sensors 592, 594, 596, and 598 are provided so that heating (by means not shown in FIG. 11) can be modulated as necessary to obtain the desired level of vapor generation from the source material. . The thermocouple 590 passes through the top wall 560 of the container at the seal 580 and terminates in an outer portion 582 coupled to a suitable controller / recorder device to assist in monitoring and controlling the steam generation operation.

[00143] FIG. 12 is a schematic diagram of a horizontal reagent delivery container 600 illustrating a solids evaporation technique according to another aspect of the present invention. The container 600 is placed in a heating jacket 610 and has a distribution valve 604 on its upper wall 602, the distribution fitting 606 being configured to couple with a distribution line 608 as illustrated.

[00144] Orienting the container horizontally in the embodiment of FIG. 12 is advantageous as long as gravity can keep the lower portion of the container wall in contact with the solid source material. As the material in contact with such wall portions evaporates, the vapors leave the walls, the solids replace the vapors, and then the solids are in the lower portion of such a horizontally oriented container. By the way, it touches the wall. In another variation, the container shown in FIG. 12 is configured to rotate about the longitudinally aligned longitudinal axis AA in the direction indicated by arrow B, thereby providing It is possible to continuously stir and mix the solid source material so that the heat of the solid in the container is uniform. In such a rotation scheme, a suitable rotary seal and coupler of the type known in the art that allows fluid sealing with a rotating member can be used in the container.

[00145] FIG. 13 is a schematic diagram of a reagent delivery system 620 according to another embodiment of the present invention comprising a buffer band.

[00146] The system 620 is encased in a heating jacket 624 and is a flow control unit that is a schematic representation of components such as mass flow controllers, valves, orifices, sensors, etc. that are or are desirable to operate the system. A container 622 with a distribution valve head 686 configured to distribute solid source material vapor into a distribution line 688 including 694 is provided. From the flow control unit 694, steam generated from the solid source material flows into the conduit 698 and enters a steam utilization unit, eg, a semiconductor processing facility.

The system 620 of FIG. 13 includes a buffer container 692 that is connected to a distribution line 688 by a conduit 690. The conduits and distribution lines may be valved and configured to allow steam to flow into the buffer container 692 during dispensing operations as needed, provided that the amount of steam dispensed is such a buffering function. It is a case that is suitable for. The buffer vessel is, of course, suitably insulated and / or heated to hold the vapor as a fluid and prevent the vapor in the buffer vessel from condensing and solidifying.

[00148] In this way, the buffer amount of the solid source material vapor is accumulated in the buffer container, and the remaining amount of the vapor in the distribution pipe 688 has become low or has to be replenished in some other form. In some cases, it can be used to back flow into the distribution line 688. The function of distributing the buffer volume of steam to the distribution line 688 can be configured in a controllable manner by appropriately sensing and monitoring steam generation in the container 622 and / or steam consumption in the steam utilization unit 698.

[00149] FIG. 14 is a perspective view of a reagent delivery container 702 inserted into an adaptively shaped heating jacket 710 illustrating another aspect of the invention in another embodiment.

[00150] The system 700 shown in FIG. 14 includes a container holding a solid source material to evaporate. Container 702 includes a distribution valve 704, thermocouples or other temperature sensing 706 and 708 on the container wall as illustrated.

[00151] Container 702 is shown lowered into the direction indicated by arrow G and into heating jacket 710. The heating jacket 710 defines a cavity 716 where it receives the container 702. The jacket is formed to mate with the container, and for such purposes, the heating jacket can have a molded insert that can conform to the outer surface of the container. The heating jacket includes a seam that can be opened by hand to facilitate insertion of the container into the cavity of the jacket. After the container is placed in the jacket, complementary mating sealing elements 720 and 722, such as Velcro® hook and loop fastener elements, engage to hold the container in place in the jacket.

[00152] The jacket includes monitoring elements associated with thermocouples or other temperature sensing elements 712 and 722, or elements 706 and 708 on the vessel wall, as shown in the figure, whereby steam generation and distribution During operation, heating by the jacket of the container can be maintained at an appropriate level to evaporate the solid source material in the container.

[00153] The heating jacket 710 is shown as being coupled to the heating regulator unit 726 by a wire 724, which is further connected to a suitable power source by a power cord 730. The heating regulator unit 726 is a programmable unit that can be preset to execute a heating cycle program of a desired duration or time interval, and such unit includes other sensors, monitoring and control in the system. It can be integrated with the equipment to allow highly efficient evaporation of the solid source material to generate steam.

[00154] FIG. 15 shows a reagent delivery container according to another aspect of the present invention, showing an associated monitoring and control component comprising a recovery manifold member coupled to a porous recovery tube to release vapor from the container. 1 is a perspective view showing a partial cross section of a system 800 that includes 802. FIG.

[00155] The system of FIG. 15 includes a cylindrical container 802 mated with a manifold cover 804. Manifold cover 804 defines a hollow interior volume and on its upper surface 810 is a distribution line for the discharge of steam that is contained in a container, e.g., derived from solid source material 806 in the form of particles as shown in the figure. A distribution valve 812 is attached to which a distribution fitting 816, shown in the figure as connected to 820, is coupled.

[00156] The container 802 includes a porous tube 808 coupled with a manifold cover 804 so that after heating the solid source material 806 in the container (heating means not shown in FIG. 15), the vapor is Flows through the wall of the porous tube and flows further upward, as indicated by arrow I, into the hollow interior volume of the manifold cover 804, after which the valve 812 is opened for fluid distribution from the container. Exhaled.

[00157] The container 802 further includes an inlet 822, which can be used to fill the container with a solid source material and then seal. The container includes a pressure sensor 826 connected to a pressure transducer (PT) 830 by a signal transmission line 828, and the pressure transducer is connected to the CPU 834 by a signal transmission line 832. CPU 834 is then connected to monitor 838 by cable 836 and can visually display data indicating the pressure in the container. Alternatively, sensor 826 may be a temperature sensor and pressure transducer 830 may be replaced with a temperature transducer.

[00158] As shown in the figure, the porous tube 808 is connected to a heating controller 842 having a function of heating the porous tube to a desired temperature by applying an appropriate electric input to the porous tube through an electric resistance heating wire 840. Can be connected. The heating controller is energized as appropriate (power supply is not shown in FIG. 15) and is connected to the CPU 834 by a signal transmission line 844 so that the system can be comprehensively monitored and controlled.

[00159] Thus, the porous tube 808 is heated to an appropriate temperature, the solid source material in the container is heated, and the resulting vapor flow is induced to flow through the internal passage of such a tube, The manifold cover 804 is sent to the collection manifold.

[00160] In another mode of operation, the heating of the porous tube 808 by the heating controller, as opposed to direct sublimation, melts the solid source material if it is susceptible to melting, resulting in a liquid transpiration flow. Can pass through the wall of the porous tube 808, and then a sufficient amount of energy is input via the resistance heating wire 840 to pulse the porous tube, and the internal passage of the hollow tube 808 The liquid inside can be vigorously vaporized. The pressure sensor 826 is then used to sense the resulting pressure and determine the remaining solid source material in the container as a function of the vapor pressure sensed by the pressure sensor. The amount can be monitored and the container 802 can be changed or the operation can be terminated at an appropriate point in the operational cycle.

[00161] FIG. 16 illustrates that the elongate support member 906 is coated with a solid source material so that the coated article is passed through the heating zone 900 so that the solid source material evaporates and is used for the fluid utilization device 932. FIG. 2 is a schematic front sectional view showing a case where steam is formed.

[00162] The heating zone 900 includes an enclosure 902 that encloses an internal volume 904. The heating zone can be of any suitable type, such as a heating furnace, oven, hot box, thermal chamber, and the like.

[00163] The elongated support member 906 in the system may be, for example, a tape, a web, a sheet, a filament, a wire, or other substrate article, and is coated with a powder coating of solid source material particles. The In the following description, the support member 906 is considered to be a tape having a respective top surface 907 and bottom surface 909.

[00164] The support member translates to a spray head 924 configured to spray powder supplied from the powder reservoir 914 to the spray head in the conduit 922, and the powder reservoir 914 to the conduit. Passes through an array of spray heads including a spray head 920 configured to spray powder supplied to the spray heads in 916. For this purpose, the powder is a solid source material coating 911 on the top surface 907 of the tape and a solid source material on the bottom surface 909 of the tape as the coated tape translates through the heating zone 900. When the coating 913 is evaporated, it is in the form of particles of a solid source material that is a source of vapor (heat introduction into the inner volume of the heating region is indicated by a heat input arrow Q).

[00165] As a result, the vapor derived from the coating of the solid source material is collected in the internal volume of the heating zone 900, passes through the discharge line 930, and can include, for example, a semiconductor manufacturing facility downstream. Enter 932.

[00166] Thus, the respective coatings on the top and bottom surfaces of tape 906 are removed by evaporation in heating zone 900 and returned to the uncoated state, the resulting tape is indicated by arrow X from the system. Translate in the direction. The tape can be a cobweb-like or sheet-like raw material that has been processed through a coating and heated evaporation zone of discontinuous length, or alternatively, the tape can be formed into an endless loop This causes the tape after passing through the system schematically shown in FIG. 16 to be returned to the coating zone and recoated with the solid source material powder.

[00167] Prior to entering the heating zone 900, a solid source material powder is prepared with a volatile binder or carrier or other matrix material to facilitate coating operations, based on consistency and structural integrity. It can be applied to a powder-coated film on a material article. Alternatively, the substrate article can be formed of a material with inherent low tack properties to which the solid source material powder adheres. As yet another alternative, the substrate article can be coated with a low tack polymer or other adhesive medium to facilitate adherence of the solid source material powder to the surface of the substrate article.

[00168] FIG. 17 shows the coating of a solid source material surface coating, adsorbed particles in a mixture where the mass of particles is subjected to energy (indicated by arrows 1010) that mediates evaporation of the solid source material 2 is a schematic cross-sectional view showing a lump 1000 of highly thermally conductive particles and a part of adsorptive highly thermally conductive particles. The adsorbed particles 1002 in the lump 1000 are coated with a coating 1004 of a solid source material in the form of a thin film, for example. The high thermal conductivity particles 1006 in the lump 1000 are provided with a coating 1008 of a solid source material in a thin film form, for example.

[00169] With such a configuration, the adsorbed particles and the high thermal conductivity material particles in the lump 1000 have a high surface area to volume ratio of the solid raw material, and only exist in the form of a thin film on the surface of the adsorption and high thermal conductivity particles. Not only does it exist in the porous form of the adsorbent, it evaporates efficiently and easily.

[00170] The particles in the mass 1000 can be coated by any suitable method, such as roller coating techniques, spraying, dipping, fluidized bed coating, or other methods that apply a coating to the particles. The adsorbent may be of any suitable type, for example, activated carbon adsorbent, molecular sieve, diatomaceous earth, viscosity type adsorbent, macroreticulate resin, silica, alumina and the like. The highly thermally conductive particles in the mass can be a highly conductive material, but are preferably formed of, for example, a metal such as nickel, stainless steel, titanium, or a highly thermally conductive ceramic.

[00171] FIG. 18 is a schematic diagram of a conveyor system 1020 for translating solid source material particles 1030 through a heating zone 1022 to evaporate the solid source material and form steam for use in a steam utilization process. It is.

[00172] As illustrated in FIG. 18, a supply container 1026 containing particles 1030 forms a reservoir for picking up particles by a conveyor 1024 with flaps, scoops, or other pick-up structures on the major surface. . Conveyor 1024 translates in the direction indicated by arrow 1032 and passes through heating zone 1022, where particles 1050 carried by the conveyor evaporate at least partially in such a heating zone and vaporize. Generate. Steam is expelled from the heating zone 1022 in the conduit 1060 and is used later.

[00173] The partially evaporated particles 1052 are conveyed to a collection chamber 1054 by a conveyor. The recovery chamber 1054 can be configured to have a supply relationship with the supply vessel 1026, and the particles are recirculated through the heating zone 1022 so that they are finally completely evaporated by the cycle passage.

[00174] Alternatively, the particles in the system of FIG. 18 are shown in the figure and described with reference to FIG. 17, for example, coated herein with a solid source material. Type of substrate particles.

[00175] FIG. 19 is a schematic illustration of a fluidized bed system 1100 for generating steam from a solid source material coated on substrate particles and utilizing the resulting steam in a downstream fluid utilization facility 1134. .

[00176] The system 1100 comprises a fluidized bed container 1102 that surrounds an internal volume 1104 having a fluidized bed 1106 of particles on a screen support 1108. Below the screen support 1108 is a gas distributor 1112 disposed in the lower plenum space 1110 of the container. Distributor 1112 is connected to a supply source 1116 of fluid gas, eg, air, collected in intake line 1118 by gas supply line 1114 and then flowing into vessel 1102 in line 1114 for purification and compression. .

[00177] Container 1102 is connected to supply hopper 1120 so as to have a solid supply relationship, from which particles coated with solid source material flow into fluidized bed 1106 through chute 1122. A take-out chute 1124 is provided on the opposite side of the fluidized bed and connected to a recovery hopper 1126 from which solids used are disposed in line 1128 for processing, regeneration, or other form of disposal. Can be removed.

[00178] Vapor derived from the evaporating solid source material produced from a fluidized bed, operating at a high temperature suitable for evaporation, is exhaled from a fluidized bed vessel in line 1132 and fluid is utilized in that line. Flow to facility 1134.

[00179] With the configuration shown in FIG. 19, the residence time of the solid source material coating particles in the hot fluidized bed can be controlled to maximize steam generation in a thermally efficient manner.

[00180] FIG. 20 is a schematic diagram of a steam generation system 1200 using solid source material, equipped with various monitoring and control components as accessories.

[00181] As shown in FIG. 20, the steam generation system 1200 includes a steam generation vessel 1201 having a floor 1202, a cover 1206, and an enclosed side wall 1204 defining a sealed interior volume 1212 therein. Such internal volume 1212 includes a quantity of initially solid source material 1218 that may be liquid or semi-solid, for example, due to heating of the solid source material (the heating means is shown in FIG. 20). Not) As shown in the drawing, the solid source material 1218 is superposed by a porous plate member 1216 fixed to the lower end of the shaft 1214.

[00182] In the configuration shown in FIG. 20, the shaft 1214 may be hollow so that steam flows through it to the high conductivity flow control valve 1260 and is expelled from the valve 1260 to the conduit 1264. Steam flows into line 2164 and enters flow regulator 1266, from which steam flows into line 1270 and into flow summing device 1272 and then into line 1274, where fluid utilization or processing equipment to go into. The flow regulator 1266 can be of any suitable type including, for example, a flow regulating valve, a mass flow regulator, a flow restriction orifice element, a fluid pressure regulator, and the like.

[00183] The flow summing device can be used to determine the cumulative amount of steam flowing from the container 1201, thereby generating an output indicating the amount of raw chemical remaining in the container. Can do. This summing device is running out of raw chemicals in the container and the container needs to be refilled with fresh raw chemicals or otherwise changed to fresh containers containing raw chemicals And can be configured to output a signal, eg, an audible and / or visual alarm.

[00184] In addition to the summing device, the level of source chemicals in the container 1201 can be determined by various methods within the system of FIG. The system can have, for example, a side chamber 1246 that is coupled in flow communication with the container 1201, where the source material 1248 is held in a semi-solid form that is liquid or flowable by heating, and a heating jacket. 1250 supplies the side chamber. The float sensor element 1252 is disposed in the side chamber and is operatively connected to a central processing unit (CPU) 1240 by a signal transmission line 1254, and signals from the float sensor to monitor the level of raw material in the side chamber. Can be sent to the CPU.

[00185] The CPU may be of any suitable type, such as a general purpose programmable computer, a microprocessor unit, a programmable logic controller, and the like. Connected to the CPU 1240 in an output relationship with the signal transmission line 1242 is an output display 1244, which provides a graphical output of visual data, such as a graphical display of the container 1201 indicating the level of the raw chemical in it. Is generated.

[00186] As another method for monitoring the level of the raw chemical substance in the container 1201, a laser signal generator 1208 that emits a laser signal can be attached to the lower side of the cover 1206 of the container. The laser signal emitted from the generator 1208 hits the upper surface of the plate member 1216, is reflected, and enters the photoelectron detector 1210 on the lower surface of the cover 1206. In response to this, the photoelectron detector 1210 transmits an output signal indicating the distance from the detector to the upper surface of the plate member to the CPU 1240 via the signal transmission line 1256, thereby monitoring the level of the raw chemical substance, Output as a graph on the monitor 1244 and / or maintain a level data log and generate an output indicating whether the source chemical in the container 1201 is running out.

[00187] In another variation for level sensing the source chemical in the container 1201, the container is mounted in a side wall 1204 of the container and is connected to a CPU 1240 operatively connected by a signal transmission line 1230. Proximity switches 1221, 1222, 1223, 1224, and 1225 that are arranged at intervals may be provided. Each proximity switch is activated by contacting or approaching the plate member 1216, and when the plate member is gradually lowered while dispensing steam from the container, the plate member is lowered to each of the successively lowering switches. Is operated, and a corresponding signal indicating such a position is transmitted to the CPU, so that the output can be monitored and the output can be transmitted, and the position of the plate member in the container can be notified to the operator. Furthermore, this makes it possible to refill the container with fresh raw material chemical substances or to replace the container with a fresh container in a timely manner.

[00188] The system 1200 further includes a dynamic inspection assembly for examining the level of source chemicals in the container when steam is not actively distributing from the container to the downstream fluid utilization process. A source 1276 of an inert gas, such as nitrogen, helium, argon, etc., is connected to a supply line 1278 pump 1280 that is placed in a supply line 1290 with a mass flow regulator 1282 therein. It functions to inject a mass of inert gas, and then the inert gas is injected into the internal volume 1212 of the container 1201. The pressure transducer 1220 is mounted on the container cover 1206 and is connected to the CPU 1240 by a signal transmission line 1262.

[00189] In operation, the pump 1280 is operated to pulse (inject) a known volume of inert gas from the source 1276 into the container 1201. The pressure transducer 1220 can then be used to determine the available open volume in the container, which is related to how much of the source chemical remains in the container, which allows the CPU 1240 to It can be output as needed.

[00190] Alternatively, the system is such that the volume of inert gas from source 1276 required to increase the pressure in container 1201 (measured by transducer 1220) to a particular pressure is determined. And the volume value of the inert gas can be input to the CPU 1240 to determine the amount of source chemical remaining in the container. In this method, a mass flow controller 1282 can be used to meter an inert gas into the container.

[00191] In any of the level determination methods described in the last two paragraphs, the determination is made when steam is not actively being supplied from the container in the dispensing mode. For this purpose, the inert gas is injected while the container 1201 is off-line. This can be done by a cycle timer program managed by a CPU connected and operating in a control relationship with the flow control valve 1260 to close the valve 1260 when dynamic level determination is made. . Discharge line 1274 may be equipped with a surge tank or other hold-up vessel (not shown in FIG. 20) in communication with this line to suck up excess volume during active dispensing operations. Thus, during dynamic level testing, valve 1260 is closed and steam from the hold-up vessel is supplied to the downstream fluid utilization process, thereby maintaining the continuity of the steam dispensing operation. The hold-up vessel can be associated with the discharge line 1274 by a suitable valve manifold, bypass line, or other fluid circuit for performing such operations.

[00192] Thus, the present invention provides an efficient and reliable apparatus and method for delivering steam from a solid source material, and the present invention provides a fluid in a way that makes steam safe and effective. It will be appreciated that it can be implemented in a variety of embodied configurations, including monitoring and control of dispensing operations, as provided to a utilization facility or process.

[00193] In other embodiments, the solid source reagent delivery system includes a container that defines an enclosed internal volume in which the solid source material is retained. The container comprises at its upper end a valve assembly wrapped by a block of a high thermal conductivity material such as aluminum that can be removably secured to the valve assembly. The block can be separated into a plurality of component parts that are joined together to form an encapsulated block structure around the valve.

[00194] For example, the block of one embodiment is formed of two half sections that enclose a valve assembly that is in thermal contact with the valve structure, so that when heated, the block is more thermally conductive when heated. Heat is transferred to the valve, preventing condensation of the solid source reagent vapor within the valve assembly.

[00195] The individual parts of the block may be coupled together in any suitable manner. For example, open and fit around the valve head assembly, after which the half sections fit together and are closed so that they can be locked in place by a suitable fastening structure, forming a block as a half section joined together with a hinge can do.

[00196] The securing structure may be of any suitable type including coupling elements, locking structures, latches, keyed structures, and the like. The block can include a passage through the block such that the source reagent vapor flows from the valve in the valve assembly through the block to the associated fluid circuit. This fluid circuit can then be combined with downstream processing equipment where the dispensed steam is used.

[00197] For such purposes, the block includes a fitting that mateably engages a valve port in the valve assembly and engages the block with an associated fluid circuit, eg, the block. Fittings, couplers and the like that allow coupling with the discharge conduit can be provided.

[00198] The block causes radiant heat, resistance heating of the block itself when combined with a suitable power source, heat generation to prevent condensation of the raw material reagent vapor in the passage of the valve and associated fluid circuit Microwave or ultrasonic energy impingement on the block, covering the block with a heating jacket configured and operated to heat the block to a high temperature, or to transfer heat to the valve passage in the valve assembly of the solid source reagent dispensing system It can be heated by a suitable heating structure including other suitable heating structures that can increase the temperature of the block.

[00199] In another aspect, the present invention relates to a solid source reagent delivery system that includes a flange used to close a container of the delivery system, provided that the flange is removed, such as a non-standard driver. It is fixed to the reagent supply container by a non-standard screw that requires a special tool. In this way, the reagent delivery system is imparted with tampering or tamper resistance characteristics.

[00200] In other embodiments, the screws used to secure the flange to the container are labeled, and these labels must be broken when utilizing the fasteners underneath. . With such a configuration, it is possible to easily detect unauthorized or unauthorized use of the container.

[00201] In yet other embodiments, the solid source reagent delivery system includes a container that defines an enclosed volume that holds the solid source material, the container being, for example, a thin cylindrical resistance heater or other It is adapted to use a cartridge heater in the form of a compact shaped heater. For example, one or more, e.g., 3 or 4 heaters, are valves associated with the vessel that are used to control the flow rate of solid source vapor exiting the vessel when the source material is heated in the vessel. It can be placed in or near the valve. The valve may be highly conductive and is a flange used to define an internal closed volume of the source with which the solid source reagent is stored and from which the solid source reagent vapor is dispensed during the dispensing operation. Or it can be mounted on another sealing member.

[00202] In one embodiment of a solid source reagent delivery package comprising a conductive block surrounding a valve as described above, the block can comprise a drilled hole or bore in which a resistive heating element is provided. It is possible to insert and heat the block and thus the valve encased by the block. Additionally or alternatively, the container itself can be formed so that the heater can be used in or near the container wall.

[00203] For example, the walls of the container can be thick enough to form a wall pocket into which such a heater can enter, and these heaters can be selectively inserted into the pocket. The container wall can be heated so that heat is transferred to the container to heat the solid source reagent material therein. A container for such purposes can be formed of a conductive material such as aluminum or an aluminum alloy.

[00204] FIG. 21 is a front view of a partial cross section of a solid source reagent delivery package 1300, according to one embodiment of the invention.

[00205] The solid source reagent delivery package 1300 has a cylindrical side wall 1304 extending along the circumference and a floor 1306 defining an enclosed volume 1372 that holds the solid source reagent 1374 along with an upper flange sealing member 1310. A solid source reagent container 1302 is included. In FIG. 21, the solid source reagent substance is shown as being prepared as a packed substance lump in the container for the sake of clarity, but this substance is likely to generate vapor from the solid source reagent. It will be understood that it can be mounted on a support or other related structure. In one particularly preferred embodiment, the solid source reagent material is carried within the interior volume of the container by a porous metal medium in either block or monolithic form or in the form of a packing.

[00206] The upper flange sealing member 1310 includes threaded passages therein for receiving respective fasteners 1312 and 1314 that engage corresponding threaded passages in the side wall 1302. In this manner, the upper flange sealing member 1310 is mechanically tied and fixed to the container side wall.

[00207] As a fraud prevention function, the heads of fasteners 1312 and 1314 may be configured to require a non-standard screwdriver to be removed, or the use of other non-standard tools may be required Therefore, it is possible to improve the characteristics of preventing illegal use of the package.

[00208] In addition, if there is an attempt to remove the contents of the package without permission by placing adhesive labels 1316 and 1318 on the head of the fastener, the attempt may be due to a broken label seal. Detected.

[00209] The upper flange sealing member 1310 has a central opening in communication with a valve assembly 1360 contained within the block 1340. Block 1340 is formed from half sections 1342 and 1344. Each half section fits together at a seam 1346 and is joined together by a fastener 1348 on the front of the block as shown in FIG. The block 1340 can open and close the block section in a bivalve style and can be formed in a half section that is hinged to the back of the block to engage the thermally contacting valve assembly 1360.

[00210] The block 1340 may include a passage therein that communicates with a valve chamber (not shown) in the valve assembly and is connected to a valve stem 1362 (also shown in the figure). Can be translated between the fully closed position and the fully open position by rotation of the valve handwheel 1364 to distribute or contain the solid source reagent vapor, respectively.

[00211] Thus, the valve assembly is in a block that terminates at the mouth where the fitting 1368 is located for coupling to the discharge line 1370, eg, as part of a fluid circuit that can be coupled to downstream semiconductor manufacturing equipment. It is possible to communicate with the discharge passage.

[00212] To heat the solid source reagent container 1302, pockets 1320 and 1322 are formed in the side wall 1304 of such container to accept insertion of the respective heaters 1326 and 1330, as shown. Can be. The heater 1326 is disposed in the wall opening, connected to an appropriate power source by the electric wire 1328, and heats the nearby container wall by resistance heating. Similarly, the wall opening 1322 contains a heater 1330 coupled to a power source by an electrical wire 1332, which may be the same power source that supplies energy to the electrical wire 1328.

[00213] In the illustrated embodiment, block 134 further accepts insertion of heaters 1350 and 1356 that are coupled to a suitable power source using wires 1352 and 1358, respectively, to provide electrical resistance heating of the block. It is heated using a passage made by hollowing in each half section of the block. Subsequent heating of the block in this manner also heats the valve assembly 1360 and associated flow paths, thereby preventing condensation of the source reagent vapor in such passages.

[00214] Although shown as having two heaters on the container sidewall and two heaters in block 1340, the evaporation, vapor pressure, and volatility characteristics of the source reagents and solids It will be appreciated that the number of heaters used in certain embodiments of the invention can be increased or decreased depending on the ambient temperature conditions in which the source reagent delivery package is used.

[00215] FIG. 22 is a front view of a solid source reagent delivery package 1380 covered with a shrink wrap film 1382 as a safety protection and tamper-evident prevention function.

[00216] A recurring problem with the delivery of solid source reagent vapors is that it is difficult to determine when the solid source reagent material is exhausted and when a new solid source reagent delivery package needs to be introduced into the process system. There are some. Thus, the present invention, in an additional aspect, presents embodiments in which the level of solid source reagent remaining in the evaporator vessel can be easily determined.

[00217] In one embodiment, the level of the source reagent material in the source container is monitored by pressure measurement. In such a method, the solid source material is heated to increase the vapor pressure while monitoring the heating vacuum gauge, manometer, and pressure to produce an output indicating the remaining amount of solid source reagent in the supply container. Use a functional converter.

[00218] A vacuum gauge can be installed at the outlet of the evaporator package to monitor the vapor pressure at the existing process temperature in the steady state system. As material is dispensed from the evaporator vessel, the available pressure is reduced to a steady state value, assuming that the pressure can be measured by a provided pressure monitoring component. Thus, steady state values of different pressures at a particular temperature can be obtained when the flow rates of the dispensed steam are different. As the evaporator temperature increases, the steady state value of the pressure also increases. Users typically use the evaporator at a fixed or constant temperature level. Thus, the steady state pressure for a given flow rate of source reagent vapor can be readily determined.

[00219] Once the material is removed from the evaporator vessel, the surface area of the material that was in contact with the heated evaporator vessel (eg, between the solid source material and the heated support structure in the heated wall or vessel). Is reduced by contact). As a result, the steady state pressure begins to decrease at a given flow rate and temperature as the level of material begins to approach depletion. Thus, the steady state pressure drop can be correlated to the amount of residual material in the evaporator vessel.

[00220] For example, the solid source reagent may be B ₁₈ H ₂₂ . When such a substance evaporates, it is necessary to gradually raise the temperature of the evaporator container in order to maintain a constant flow rate of the raw material reagent vapor. This is due to the fact that the vapor pressure of the raw material decreases as the material evaporates. This can occur due to a variety of causes, such as a reduction in total surface area, isomerization or decomposition of the solid source reagent material. Between the amount of material remaining in the evaporator vessel, the vessel temperature, and the open rate characteristic of the regulator valve required to maintain a given flow rate or a given pressure downstream of the flow regulator valve on the evaporator vessel. Functional relationships can be determined from experience.

[00221] In other embodiments, the amount of source reagent material remaining in the evaporator vessel is determined by applying a predetermined amount of heating energy to the evaporator vessel within a specified time period. The rate at which the system reaches equilibrium vapor pressure can be correlated to the material remaining in the evaporator vessel. This can establish an empirical relationship that relates the speed approaching the equilibrium pressure to the amount of material remaining in the evaporator vessel.

[00222] The evaporator vessel and upper flange sealing member may be formed from any suitable material capable of heating the source reagent material to generate sufficient reagent vapor for distribution to an external use location.

[00223] In one embodiment of the general type raw material reagent delivery package shown in FIG. 21, the container is formed of aluminum that provides high thermal conductivity capable of heating the raw material material, and the valve assembly and top. The flow control valve in the flange sealing member is made of stainless steel. In such a system, the container can be insulated so that only the valve is heated. Heating only the valve ensures that the temperature of the valve is always higher than the temperature of the solid source reagent material in the container. By processing the raw material reagent container from a material such as aluminum, the uniformity of heat with respect to the contents of the container is increased. The stainless steel upper flange sealing member has some resistance to heat transfer, so that the source reagent container is at a lower temperature than the valve assembly and solids do not solidify inside the valve. Heat is input to the valve by a block of the type shown in FIG. 21, and the heat is transmitted through the stainless steel flange sealing member and reaches the remaining portion of the raw material reagent container.

[00224] In other embodiments, the present invention solves problems associated with very low vapor pressure (at room temperature) solid feed reagents, such as B ₁₄ and B ₁₈ H ₂₂ , and some indium and antimony solid feeds To do. Because of the very low vapor pressure, these materials must be heated so that steam can be delivered, but it is difficult to provide sufficient heating to generate the required amount of steam.

[00225] In such a case, in the present invention, a solvent in which the raw material reagent solids are dissolved is used to increase the evaporation rate of the low vapor pressure solids when the solvent evaporates. The solvent can also be used to carry the low vapor pressure solids to a point of use where the solvent and the low vapor pressure solids are instantly evaporated.

[00226] When using a solvent to dissolve a low vapor pressure solid, use an appropriate solvent, including an organic solvent as well as an inorganic solvent (which does not react with the solid) to increase the rate of solid evaporation. Can be increased. The solid vapor can then be extracted from the solvent and flow to the point of use. Alternatively, a solvent containing dissolved solids is flowed to the evaporator where the solvent / raw reagent mixture is flushed and the resulting vapor is removed from other processes, such as deposits that can be removed by the raw reagent vapor. Use as needed to clean the system room.

[00227] In other embodiments, the present invention implements techniques for monitoring solid source reagents to determine when such materials are approaching depletion in source reagent supply containers. In this embodiment, a heat flux sensor is used to determine residual solid chemicals remaining in the source reagent supply container. Since the chemical substance is heated and evaporated at the time of use, the measurement result of the heat flux can be used to monitor the level of the raw material reagent remaining in the raw material reagent supply container.

[00228] A suitable heat flux sensor is commercially available and is readily available. In one embodiment, the heat flux sensor is a thin film thermocouple converter that generates a voltage that is proportional to the heat flux through the sensor element and can be directly correlated to the actual heat flux. This type of heat flux sensor is described by Omega Engineering, Inc. (Stanford, Conn.) And are sold as Model HFS-3 and Model HFS-4 Thin-film Heat-Flux Sensor.

[00229] The heat flux can be constantly monitored by mounting the heat flux sensor on the raw material reagent supply container. In steady state operation, the heat flux typically has a relatively low value when the supply vessel is insulated, especially as desirable, with minimal heat loss from the vessel. However, when chemicals are exhausted, the necessary thermal load on the supply vessel is reduced over time, since less material is maintained at an appropriate level to generate the vapor for distribution. More importantly, heat loss occurs on the surface of the solid chemical inside the container, and as the solid chemical evaporates, heat is lost from the surface of the solid, and the temperature in such areas decreases slightly. That is. As the rest of the environment becomes hot, heat flow to the solid surface is induced and this flux is measured and monitored using a heat flux sensor.

[00230] In certain configurations, several such heat flux sensors are placed along the longitudinal axis of the supply vessel so that the level of chemicals in the vessel can be closely monitored over time. it can. As the chemical level decreases, the heat flux sensor detects a change in the heat flux at the chemical level. In most of the dispensing operations, the heat flux sensor functions in a steady state and measures heat loss due to convection from the source container to the surrounding environment.

[00231] The present invention in another aspect provides a solid source reagent delivery package that delivers reagent vapors near or below room temperature using active cooling. This method can be used, for example, to deliver xenon difluoride to the implant source chamber. At 25 ° C., XeF ₂ has sufficient vapor pressure and can flow up to a few standard cubic centimeters per minute (sccm) using a reasonable size, eg, a delivery line less than 1 inch inside diameter. However, a supply container filled with XeF ₂ may be able to deliver a sufficient flow rate only for a relatively short period, such as a few minutes. When the substance is delivered, the surface of the solid source reagent can be cooled by evaporation of the substance as described above. To solve this problem, an active cooling supply vessel can be used to maintain a temperature between 20 ° C. and 30 ° C. depending on process requirements. The container temperature is kept slightly below the temperature of the delivery line so that external heating of the delivery line is not required. In this way, the source reagent material can be delivered at a sufficiently high flow rate without placing the material in the delivery line.

[00232] There are a variety of chemicals that can be delivered using active cooling. In essence, this method is applicable to chemicals having sufficient vapor pressure to maintain an acceptable flow at a temperature between about 10 ° C. and about 50 ° C.

[00233] Using a vortex cooler can quickly cool a hot supply vessel. For example, a supply vessel used to deliver octadecaborane operates within a range of 93 ° C to 115 ° C. In order to remove the supply container after use, the supply container must be cooled sufficiently for the operator to handle, and the temperature of the container should be lowered to a handleable temperature using a vortex cooler. Can do.

[00234] FIG. 23 shows valve surface temperature (curve A), lower vessel surface temperature (curve B), ambient temperature (curve C), temperature monitored by heat flux sensor (curve D), upper supply vessel surface temperature. (Curve E), including the aluminum adapter surface temperature (curve F) of the adapter disposed between the container body and the flange sealing member, and the temperature difference (curve G) between the supply container valve and the supply container body. FIG. 4 is a graph of temperature (° C.) and heat flux sensor reading (DC volts) as a function of elapsed time (minutes) at various locations in the source reagent supply package. The vortex cooler used to generate the data shown in FIG. 23 is an Exair Model 3204 Vortex Cooler deployed for active cooling of a chemical-free supply vessel in a simple proof-of-concept test configuration. there were.

[00235] The data shown in FIG. 23 was obtained using a supply container with one loop control on the container body. In parallel circuit configurations, different wattages were added to the valve and vessel body sections. The Exair Model 3204 Vortex Cooler was operated to remove heat at a constant rate from the bottom of the feed vessel. In this test, a pressure of 50 psig was applied to the refrigerator inlet. Corresponding to about 2 standard cubic feet (scfm) of nitrogen flow at about 0 ° C., as estimated from the reference material provided by the manufacturer of the vortex cooler device (this further corresponds to about 40 watts of cooling) .

[00236] In another aspect of the present invention, the solid source reagent is exhausted in the middle of a processing operation, or the determination of the predicted consumption of the supply container is inaccurate, and the supply container stops operating early. Other arrangements for monitoring the amount of solid source reagent in the supply container are realized, which avoids the situation where a fresh reagent request container is replaced and, as a result, the solid source reagent is depleted.

[00237] Once installed, the source container is typically in a heating enclosure that is difficult to weigh the container, so the tare weight of the container can be used to determine the amount of solid source reagent contained therein. A simple weighing of the material container subtracted from the measured weight will not solve this problem.

[00238] The present invention solves such a problem by employing a small mid-infrared sensor that is in direct contact with the solid source reagent substance and mounted in the container together with the sensor head inside the enclosed volume of the container. . The sensor can be of any suitable type and can operate in the wavelength range of 2 μm to 14 μm of the infrared spectrum, for example. Preferred sensors for such purposes include Wilks Enterprise, Inc. Available from the company (South Norwalk, Conn.), Which is an in-line mid-infrared (MIR) sensor using attenuated total reflection (ATR) sampling.

[00239] In ATR sampling, the radiation is internally reflected under the infrared transmission optics, and the energy of the beam spreads slightly beyond the surface with each reflection, when the sample is brought into contact with the reflecting surface. Infrared energy is absorbed at a wavelength that the sample absorbs.

[00240] More specifically, infrared light from a continuous light source rebounds on an infrared absorbing surface coated with a source material. The solid source material is placed on an optical surface or condensed as a thin film on such a surface. Part of the light is absorbed by this thin film. As the thickness of the solid source material decreases (when solids evaporate and vapors are distributed), the infrared signal increases. If there is no more material left, an end point is reached, and such end point can be easily distinguished from the time-dependent curve. At the end point, the evaporator container can be replaced and a signal can be sent to the user indicating that it is time to introduce a fresh container completely filled with solid source reagent material.

[00241] In other implementations that use mid-range infrared sensors, IR filters are used to limit detection to the IR region that the source reagent material absorbs.

[00242] In other embodiments, multiple bands in the infrared region are monitored, thereby separately monitoring solids and unwanted degradation by-products to alert the user to composition changes.

[00243] In yet another embodiment, the material on the infrared absorbing surface is encapsulated in a mesh and is absorbed during transport and / or installation of the reagent supply container with physical vibration or mechanical shock applied to the container. It will not come off the surface.

[00244] In yet another embodiment, a mid-range infrared sensor is used to measure the amount of material dissolved in the ionic liquid storage medium, where the source reagent is dissolved in such medium. The source reagent is released from the ionic liquid storage medium under the distribution conditions and flows out of the source reagent supply container.

[00245] The present invention, in another embodiment, presents using solid XeF ₂ source material to deliver xenon difluoride chemical to an ion implantation system. This embodiment of the invention relates to an ion implanter that is contaminated during operation and requires cleaning to maintain efficient operation. A specific problem with the solid XeF ₂ source material is that it delivers enough chemical to perform the cleaning while meeting specifications for a container that fits into the gas box of the ion implanter system, and such a container is 1500 pounds / The ability to withstand accidental overpressures of square inches (psi) or greater.

[00246] The present invention is in the form of a carrier structure for a solid source material, in which a metal foam insert (s) is preferably prepared in press-fit form when providing a source reagent container processed from aluminum. Solve problems with aluminum foam insert (s). The aluminum foam forms a high surface area support structure capable of transporting heat energy into the interior region of the interior volume of the container, which provides highly efficient heat transfer and then sublimates the solid source material.

[00247] Instead of aluminum, the source reagent supply container and the foaming agent insert (s) are processed from a metal other than aluminum, such as a metal with suitable conductivity and heat capacity characteristics, such as stainless steel, nickel, bronze, etc. be able to. Instead of foam insert (s), surface area within the internal volume of the raw material container by filling with metal wool, metal spheres, sequential trays (eg in a stacked arrangement), or other packing particles or media A wide conductive support structure can be included. The filling desirably has a large surface area, high void volume, suitable thermal properties, and suitable structural integrity. When used as a filling medium, the sphere may be featured in its contents, contoured or birdcage-like, and use a geometrical shape other than a sphere, such as a cube or cylinder. In certain embodiments, such filler media particles can be formed from a metal foam.

[00248] Compared to an evaporator having a plurality of trays in the internal volume, the use of metal foam, metal wool or the like is advantageous in terms of capacity and ease of filling. Three-dimensional porous networks related to flat trays and plate-like structures result in a significantly solid source reagent volume. In addition, trays and plate-like structures must be loaded with solid source reagents one level at a time, which is a time-consuming and tedious process, but three-dimensional foaming of granular or particulate solid source reagent materials It can be poured into the body network and simply shaken to settle in place so that finely divided solids can be dispersed throughout the porous matrix.

[00249] To meet the accidental overpressure specification for deploying a solid source reagent supply container in a gas box of an ion implanter while ensuring a high level of safety, the solid source reagent supply container of one embodiment Is processed with a stainless steel conflat flange member explosively bonded to aluminum. This structure provides an aluminum-to-steel transition in an assembly that takes advantage of the strength of steel in the upper portion of the structure and takes advantage of the thermal conductivity of aluminum elsewhere in the structure.

[00250] In other embodiments, explosive crimping is used to form a structure with a steel upper portion, in this case threaded for threaded mounting of a screw-on top sealing member, thereby providing a solid raw material The structural strength of steel can be utilized in the upper part of the reagent supply container, and the high conductivity of aluminum can be utilized in the lower part of the solid source reagent supply container. Explosive crimping is a commercially available process and can be effectively used in processing solid source reagent supply containers within the broad scope of the present invention.

[00251] In many cases, the solid source reagent container and the porous foam insert (s) or other porous media contained therein are surface treated or coated with other non-fluids The chemical resistance of the container and its internal structure, which is suitable for utilizing the base chemical, can be further enhanced. For example, the container and porous medium can be polymer coated or, if formed of a material such as aluminum, anodized or passivated.

[00252] When a solid foam is used as a support, various solid source materials can be easily stored and delivered. Solid source materials for such purposes are supplied in finely divided form and are suitable for particular porous media and solid source materials in a given application, such as vibration, agitation, solution deposition, or other It can be dispersed in the foam material in an incorporated manner.

[00253] Accordingly, the present invention contemplates a solid source reagent delivery package for solid fluorine chemicals that, in a preferred embodiment, is processed to withstand pressures of 1500 psi or greater. Such package containers can be of any suitable size, for example, 3-8 inches in diameter and 10-25 inches in height. In one embodiment, the container has a diameter of 4 inches, a height of 13 inches, and an internal volume capacity> 60 cm ³ . The container of such an embodiment is formed of aluminum and includes a press-fit aluminum foam insert, and the valve and upper sealing flange member are formed of stainless steel. The valve in such a package is a manual valve with a valve conductivity Cv> 2.65, with a maximum flow rate of 15 standard cubic centimeters / minute in 1 hour.

[00254] Such a solid source reagent delivery package substantially reduces the sensitivity of the solid source reagent that undergoes evaporative cooling and surface area aggregation by placing a porous medium within the interior volume of the container. Aluminum foam is a preferred insertion media material, with 5 pores per inch (ppi) foam material being very advantageous.

[00255] The package of one embodiment includes an upper flange sealing member secured to the side wall of the container by bolt fasteners, as shown in FIG. Alternatively, the upper flange sealing member can be bolted to the side wall with bolts that run vertically through the entire length of the side wall, secured to the upper flange sealing member at the top and to the floor of the container at the bottom. In such an embodiment, the floor can be processed as a separate member, with the upper sealing member and the lowermost portion each having a gasket, O-ring, or other sealing element between it and the adjacent end face of the sidewall. Can be provided.

[00256] The upper flange sealing member of other embodiments is screwed to the inner surface so that it can be threaded onto the external threaded surface of the container, with an O-ring or gasket seal used to form a leak-proof seal, as appropriate. Can be formed as a cap. Alternatively, the upper sealing member may comprise a screw-on cap and bull plug structure, optionally with an O-ring or gasket sealing element.

[00257] In still another embodiment, the upper sealing member is a stainless steel flange member explosively bonded to an aluminum container.

[00258] FIG. 24 is a front view showing a partial cross section of a solid source reagent delivery package 1400 including a container 1402 that defines an enclosed internal volume 1404. FIG. Within the interior volume 1404, an array of vertically stacked porous metal packs 1406, 1408, 1410, 1412, and 1414 is constructed that is press fit into the interior volume 1404. Upper packs 1412 and 1414 have central bores 1416 and 1418 that define a passage 1420.

[00259] Container 1402 is formed of a metal, such as aluminum, that is selected to provide thermal conductivity that favors heat transfer to the container and the porous metal insert therein, and to generate source reagent vapor. Can do. What is explosively crimped to the container 1402 is, for example, a lower flange 1422 that can be formed of stainless steel. The upper flange 1424 is bolted to the lower flange 1422 by bolts (not shown in FIG. 24) to which nuts 1432, 1436, 1438 and 1440 are coupled. The upper flange 1424 is connected to the fitting 1426 and the flange 1430 is connected to the fitting so that the vapor distribution pipe line can be coupled to the solid raw material reagent supply container.

[00260] The porous metal insert in such a container has finely divided solid source reagent dispersed in the pores of the metal insert. By incorporating the solid source reagent into the pores of the metal foam article, steam is generated from the solid source reagent very efficiently by the heat transferred to the foam article.

[00261] Thus, the present invention provides an effective solid source reagent delivery package that is particularly useful for delivery of xenon difluoride. Xenon difluoride is a white crystalline powder having a molecular weight of 169.29 and a melting point of about 135 ° C. The change in enthalpy involved in the sublimation of xenon difluoride is about 13.315 kcal / mole, or in other words about 6 cal / min for a flow rate of 10 sccm of XeF ₂ vapor.

[00262] Preferred metal foam using xenon difluoride as a solid source reagent in packaging, 5 pores / inch in the form of substantially equal pack or disc to the inner diameter of the vessel diameter, density 0.189 g / cubic centimeter, Includes aluminum foam with a thermal conductivity of ~ 4 Watts / mK and a surface area of about 3.3 cm ² / cm ³ , whereby the disks are stacked and press-fitted into the container, and the stacked arrangement of disks within the internal volume of the container Can be formed.

[00263] In one preferred embodiment, the solid reducing reagent delivery package xenon difluoride is provided with a (plurality of) a vessel containing an aluminum foam insert into, (s) inserts, one Or it includes a plurality of packs, the heating block is in the upper part of the container and active cooling is performed in the lower part of the container to counter the surface cooling and aggregation of the solid source reagent. An active cooling function can be provided in the vortex cooling unit associated with the lower part of the vessel. By using such a package, a chamber, such as a microelectronic device ion implantation process chamber, is cleaned, and two fluorides are removed to remove deposits resulting from ion implantation of such dopants, such as boron, arsenic, and phosphorus. Xenon vapor can be distributed.

[00264] The xenon difluoride dispensed from the source reagent delivery package is exposed to plasma generation together with a carrier gas such as argon, for example, to achieve very efficient cleaning of the ion implantation process chamber over a predetermined operating time. This can be done after deposits of dopant species have accumulated in such process chambers, or in some other way to such an extent that they require cleaning of the process chambers.

[00265] For all purposes, the disclosures of US Pat. No. 5,518,528, US Pat. No. 6,089,027, US Pat. No. 6,101,816, and US Pat. No. 6,343,476 Are incorporated herein by reference.

[00266] The present invention considers providing a highly conductive valve useful for delivering low pressure fluid. The valve of the present invention has a flow coefficient that is significantly greater than the prior art valves previously used for fluid delivery in low pressure applications.

[00267] Preferably, the valve of the present invention is configured and configured to accommodate operating pressures up to 230 psig, operating temperatures ranging from -28 ° C to 150 ° C.

[00268] Another aspect of the invention relates to a substance delivery system comprising a highly conductive valve of the invention attached to a substance supply container. According to one embodiment, the substance supply container is a substance used in the manufacture of semiconductors, such as a solid material that is heated or otherwise processed in the container to form a fluid, or alternatively, a fluid to be dispensed. including. Specific examples of reagents that can be dispensed with such a configuration include, but are not limited to, organometallic reagents, etching reagents, cleaning reagents, photoresist precursor materials, and dopants.

[00269] Another aspect of the invention is for utilizing the delivered material in a semiconductor manufacturing facility, eg, in a semiconductor manufacturing facility, for applications such as ion implantation, chemical vapor deposition, etching, cleaning, etc. The invention relates to a system for use in the manufacture of semiconductor devices comprising a substance delivery system according to the invention coupled to an apparatus.

[00270] The valve of the present invention has the property of compactness, for example, the total volume (here, the total volume pointing to the total volume of the valve body, including the void volume of the valve chamber and the void volume of the connecting passage in the valve body). It has a valve body with a volume) of 4 to 20 cubic inches.

[00271] In one embodiment of the valve body, 15 to 35% of the total volume is occupied by the valve chamber (a chamber in which the valve element is movable to open and close the valve). In a preferred embodiment where the total volume of the valve body is in the range of 7 to 10 cubic inches, the valve chamber occupies a volume of 1.5 to 3.5 cubic inches. The inlet passage in the valve body occupies 0.15 to 0.45 cubic inches when measured from the intersection with the valve chamber to the inlet passage opening on the surface of the valve body, and the outlet passage in the valve body Measured from the intersection to the outlet passage opening on the surface of the valve body can occupy 0.05 to 0.45 cubic inches.

[00272] In one preferred embodiment of such a compact valve of the present invention, the ratio of the diameter of the outlet passage to the diameter of the inlet passage is in the range of 0.75 to 1.25, more preferably 0. Within the range of .80 to 1.15, even more preferably within the range of 0.90 to 1.10, most preferably the ratio is within the range of 0.95 to 1.05 .

[00273] In another aspect, the ratio of the length of the outlet passage to the length of the inlet passage of a preferred embodiment is in the range of 0.20 to 1.5, more preferably 0.3 to 1. It is in the range of 2 and most preferably in the range of 0.35 to 1.0.

[00274] Accordingly, the valve of the present invention is a small volume valve (interpreted herein to indicate a valve having a valve body with a total volume of <20 cubic inches) and has a relatively large interior. Has internal open volume. For example, the open volume of the valve (ie, the volume determined as the sum of the individual volumes of the inlet passage, outlet passage, and valve chamber) is in the range of 25 to 45% of the total volume of the valve body, more preferably It can be in the range of 30 to 40% of the total volume of the valve body.

[00275] The valve of the present invention is characterized by high conductivity and preferably has a flow coefficient greater than 2, more preferably a flow coefficient of at least 2.5.

[00276] As a specific example, a valve of the type described below with reference to FIGS. 25-28 has a flow coefficient on the order of about 2.7 to 2.9. This is in contrast to valves that are used in the prior art to distribute low pressure fluid with a flow coefficient on the order of about 0.2 to 0.35.

[00277] Considering the general operation of the valve, the flow control valve uses a change in the position of the valve element within the valve housing to limit the flow of fluid through the valve body and valve chamber containing the movable valve element, It can be seen that the fluid flow rate can be controlled by controlling the flow rate. The fluid flow control valve can control the fluid flow rate by imposing an inherent differential pressure between the fluid pressure at the valve inlet and the fluid pressure at the valve outlet separately or in addition. For a given orifice size of the valve opening, increasing the differential pressure generally affects the increase in flow rate.

[00278] The flow coefficient of the valve, sometimes referred to as the valve capacity index, is related to the flow rate and differential pressure characteristics of the valve. The flow coefficient allows the relative performance of different valves to be evaluated, so that the flow or differential pressure when one of two such variables (ie, flow and pressure drop) is known. Can be determined.

[00279] As used herein, the term valve flow coefficient C _v causes a pressure drop 1 pound / square inch on the valve, the gallons / min units at a water temperature 70 ° F Refers to the expressed flow rate. Units of the valve flow coefficient is designated by this, the value of C _v is henceforth be referenced without dimensional unit.

[00280] As used herein when referring to a valve of the present invention, the term high conductivity, the valve means having a C _v of at least 2.

[00281] The valve of the present invention has achieved substantial advancement in the art, with low pressure fluid ranging from high fluid pressure to even very low fluid pressure, for example, pressures on the order of 0.005 to 10 torr. Can be distributed.

[00282] The highly conductive valves of the present invention can be used in a variety of fluid flow applications.

[00283] In a preferred embodiment, the valve is used as a distribution control valve for the flow of source chemicals from the vessel containing it. The source chemical can be in any suitable form. In one particular embodiment, the source chemical is in the form of a vaporizable solid that is used as a source of vapor for use in semiconductor manufacturing operations. In other specific embodiments, the source chemical may be a liquid source for generating vapors used in downstream gas consuming equipment. In another particular embodiment, the source chemical is a gaseous reagent held to adsorb on a particular physical adsorption media bed from which gas is subject to flow distribution conditions to an external point of use. Is desorbed. In yet another specific embodiment, the source chemical is a fluid that is held at high pressure in a vessel with a fluid pressure regulator inside the vessel, for example as further described in US Pat. No. 6,101,816. As specifically described, the set point of the regulator allows low pressure distribution of fluid.

[00284] The valve of the present invention includes a valve body defining a valve chamber therein. The inlet passage is in communication with the valve chamber for flowing fluid into the valve body, and the outlet passage is in communication with the valve chamber for flowing fluid out of the valve body. The valve includes a valve element and an actuator assembly that allows movement of the valve element between a fully open position and a fully closed position within the valve chamber. The inlet and outlet passages, together with the valve chamber, allow fluid to flow through the valve body when the valve element is in the open position. The valve inlet and outlet passages are substantially perpendicular to each other.

[00285] Each inlet and outlet fluid flow path in the valve body is preferably generally straight, and preferably the intersection of the centerlines of each inlet and outlet passage defines a 90 ° included angle. Aligned at right angles to each other.

[00286] The inlet and outlet passages in the valve body may be of any suitable shape and cross-sectional configuration, but preferably in each case a generally cylindrical shape with a circular cross-section crossing the longitudinal centerline of the passage It is. Each passage has constituent sections with different diameters with respect to each other, but the dimensional deviation along the length of the flow path is slight in nature, avoiding hydrodynamic effects that significantly reduce valve flow conductivity Is done.

[00287] The inlet and outlet passages each terminate at a valve chamber in the valve body. The valve chamber is appropriately sized to include a diaphragm and rod assembly to seal the inlet passage in the closed position of the valve. The valve stem extends out of the valve body, and the handle, handwheel, automatic actuator, or other device or sub for moving the valve element in the valve chamber between its fully open and fully closed positions. Fixed to an operating structure such as an assembly.

[00288] In one embodiment, the actuator is a handle that can be formed with a shaped or textured surface to improve the grip of the user's hand attempting to manually actuate the valve.

[00289] Referring now to the drawings, FIG. 25 is a perspective view of a highly conductive valve according to one embodiment of the present invention.

[00290] The high conductivity valve 1510 includes a valve body 1512 having an inlet / outlet opening 1514 in which a discharge fitting 16 defining a discharge passage 1518 is disposed.

[00291] The valve body 1512 of the embodiment shown in the figure has a block-like three-dimensional structure, with the main flat side surface 1515 and the smaller flat end surface 1517 defining an eight-side block structure. The valve body may have a suitable three-dimensional structure and may be a rectangular parallelepiped, cylinder, cube, or other suitable shape.

[00292] In the embodiment of FIG. 25, a valve stem (not shown in FIG. 25) extends outwardly from the valve body to manually open and close the valve for fluid flow therethrough. Engages with a handle 1520 that can be grabbed and rotated clockwise or counterclockwise.

[00293] The valve body 1512 can be formed of a suitable material suitable for fluid dispensing applications. In a preferred embodiment, the valve body is a single machined block of stainless steel, 316L. In other specific embodiments, the valve body may be aluminum, hastelloy, nickel, carbon steel, or other suitable suitable for reagents dispensed by the valve, temperature, pressure, and other processing conditions involved in the operation of the valve. It can be formed from a constituent material.

[00294] The valve is formed of a material that imparts an operating pressure range and operating temperature range characteristic to the valve that is compatible with the particular end use in which the valve is used. In one embodiment of the present invention, the operating pressure range of the valve is in the range of up to 230 pounds per square inch gauge (psig) pressure and the operating temperature range is from -28 ° C to 150 ° C.

[00295] The discharge fitting 1516 may be any suitable type suitable for coupling to a fluid circuit or other component of a fluid distribution system. The discharge fitting of one embodiment of the present invention is a male VCR fitting. The handle 1520 can be formed of a suitable material, such as a polymer material, metal, ceramic, composite material, etc., for example, a polyester material.

[00296] FIG. 26 is a plan view of the high conductivity valve 1510 of FIG. 25, showing the overall configuration of the handle 1520 and the male VCR fitting 1516 attached to the valve body.

[00297] FIG. 27 is a front view of the valve 1510 of FIGS. 25 and 26, showing further details of its construction.

[00298] Portions and features of valve 1510 as shown in FIG. 27 are numbered to correspond with respect to the same or corresponding structure in FIGS.

As shown in FIG. 27, the tube stub 1522 is secured to the bottom surface of the valve body 1512. The tube stub is coaxial with the inlet passage in the valve, as described in more detail below with reference to FIG. The tube stub 1522 can be secured to the valve body by welding, brazing, or other suitable connection method or technique.

[00300] In one embodiment, the tube stub 1522 is surrounded by a flange element 1526 as shown by the dotted outline in FIG. Such flanges form a coupling structure or other cooperating structure for connecting the valve to the mating flange and operate by positioning the valve for flowing fluid into the opening 1524 of the tube stub 1522 during dispensing operation. Can be used to let The flange 26 can be coupled to the valve body 1512 by welding, brazing, or other connection methods.

[00301] In other embodiments, such a flange can be machined with the valve body from a single piece of metal stock. In such a single machined configuration, it is possible to eliminate the pipe stub and machine the inlet passage through the flange and into the valve body.

[00302] FIG. 28 is a cross-sectional front view of the valve 10 of FIGS. 25-27, taken along line AA of FIG.

[00303] As illustrated in FIG. 28, a tube stub 1522 is secured to the bottom surface of the valve body 1512 and defines an internal passage 1524 that communicates with inlet passage segments 1552 and 1550 in the valve body. As already explained, the difference in diameter between the passage sections 1550 and 1552 is desirably small and does not unduly interfere with fluid flow. In the illustrated embodiment, the passage segment 1550 is slightly larger in diameter than the passage segment 1552, the latter being on the order of about 0.37 inches in diameter and equal to the diameter of the inlet passage in the tube stub 1522. Preferably, the ratio of the diameter of passage segment 1550 to the diameter of passage segment 1552 is in the range of 0.995 to 1.005.

[00304] The inlet passage formed by passage segments 1550 and 1552 is potentially in communication with the valve chamber 1536. The valve chamber 1536 is formed as a cavity in the valve body 1512. The valve chamber 36 is also in communication with an outlet passage 1534, which has a specific embodiment diameter of about 0.37 inches to match the same diameter bore in the male VCR fitting 1516. Preferably, the ratio of the diameter of the outlet passage 1534 to the diameter of the bore in the male VCR fitting 1516 is in the range of 0.995 to 1.005.

[00305] As illustrated in FIG. 28, the inlet passage formed by passage segments 1550 and 1552 is the outlet passage 1534 (and the associated discharge passage 1518 of the VCR fitting 1516 that is coaxial with the outlet passage 1534). The vertical center line YY is perpendicular to the vertical center line XX. According to the present invention, the inlet passage of the valve is perpendicular or “substantially perpendicular” to the outlet passage of the valve. The phrase “substantially vertical” means within 5 degrees of vertical.

[00306] In the valve chamber 1536, the valve includes a gasket 1540 that fits in conjunction with the diaphragm / rod subassembly 1542 in the position shown in FIG. 28 and closes the valve against flow. Diaphragm / rod subassembly 1542 is coupled to bonnet 1544 and actuator bearing assembly 1546 and includes a valve stem 1533 that extends upward from the top surface of valve body 1512 and engages handle 1520.

[00307] The handle 1520 is secured to the valve stem 1533 using a handle positioning screw 1530 in the threaded opening 1532 of the handle. The set screw holds the handle in place to manually actuate the valve, thereby translating the diaphragm / rod assembly between the fully open and fully closed positions within the valve chamber 1536.

[00308] Accordingly, in the position shown in FIG. 28, the diaphragm / rod subassembly 1542 and associated gasket maintain a sealing action against the inlet passage segments 1550 and 1552 and the inner passage 1524 of the tube stub 1522. If fluid is desired to be dispensed, the handle 1520 is rotated appropriately about the longitudinal axis YY to retract the diaphragm / rod subassembly from the top of the inlet passage and the inlet passage segments 1552 and 1550 in the valve body and valve chamber 1536. Through the fluid to the outlet passage 1532. The outlet passage 1532 communicates with the discharge passage 1518 of the male VCR fitting 1516 and then flows the dispensed fluid to a fluid circuit, manifold, or other location where the dispensed fluid is used or used.

[00309] When performing a dispensing operation, fluid flows vertically upward through the valve body, enters the valve chamber 1536, changes direction horizontally and communicates with the discharge passage 1518 from the valve body in the outlet passage 1534. Flows out.

[00310] Such “normal flow” of fluid through the valve body is unexpectedly superior with respect to lateral flow through prior art fluid distribution valves. As indicated above, the valve of the present invention may take the valve flow coefficient C _v of about from about 2.7 2.9 In a particular embodiment. This is in stark contrast to the performance of a conventional corresponding prior art valve with a conventional end-to-end flow through the valve body that has a flow coefficient of about 0.2 to 0.3, for example. It is.

[00311] The valve 1510 may be any size that is suitable for the end use in which it is used. In one embodiment, the valve body 1512 and associated handle 1520 together have a height (H + K) on the order of about 3.2 inches, and the valve body itself has a height (H) of about 2 inches. The valve body 1512 in such an embodiment has a generally square shape with respect to the major surface, and the dimension of each side is on the order of about 1.875 inches (W). In such an exemplary valve, the fluid discharge passage 1518 of the male VCR fitting 1516 has an inner diameter on the order of 0.37 inches, the diameter of the tube stub 1522 (D ₁ ) and the diameter of the inlet passage segment 1552 (D ₁ ). The diameter of the inlet passage segment 1550 (D ₂ ), the diameter of the outlet passage 1534 (D ₃ ), and the diameter of the fluid discharge passage 1518 (D ₄ ) are preferably within 10% of each other.

[00312] The highly conductive valve of the present invention has achieved substantial progress in the field, and is superior to the flow control valves used so far. By using the valve of the present invention, it is possible to perform fluid distribution at a high flow rate in a low-pressure use form, and it is very advantageous for application to a fluid storage and distribution container in which a high degree of gas utilization is desired.

[00313] FIG. 29 shows that a heating jacket is arranged to heat according to the required amount of fluid in the semiconductor manufacturing facility, in fluid communication with the fluid circuit to deliver the fluid to the semiconductor manufacturing facility. 1 is a schematic representation of a configured solid source reagent storage and dispensing container 1570 incorporating a highly conductive valve 1510 of the present invention.

[00314] As shown in FIG. 29, the high conductivity valve 1510 includes a valve body 1512 with which a manually actuated handle 1520 is associated. Discharge fitting 16 is shown as having an outlet for expelling fluid. Valve 1510 is coupled to the neck of a solid source reagent storage and dispensing container 1570 containing a suitable solid source reagent, such as decaborane or octadecaborane. The lower portion of the container 1570 is disposed within a heating jacket 1572, illustrated as an electrical resistance heating jacket that is connected to the heating regulator unit 1578 by wires 1574 and 1576. The heating regulator unit 1578 is connected to a suitable power source (not shown) by a power cord 1580 and provides electrical inputs for providing a desired level of heating to evaporate solids in the container 1570 and wires 1574 and 1576 can be selectively adjusted to be sent to heating jacket 1572 via

[00315] Discharge fitting 1516 is illustrated as being coupled to a fluid circuit schematically illustrated by lines 1582 and 1586 and a flow control unit 1584. A flow control unit, as schematically shown in the figure, is a mass flow regulator, pressure transducer, surge tank, pump, compressor, as may be necessary or desirable in the technique of dispensing fluid reagents from containers 1570. Represents a suitable flow instrumentation, such as a flow control valve, sensor, moving fluid drive, etc.

[00316] Fluid circuit line 1586 is connected to a semiconductor manufacturing facility 1588, for example, which may be conveniently supplied with fluid from an ion implantation facility, chemical vapor deposition facility, photoresist etch facility, or vessel 1570. Other fluid utilization units.

[00317] The system schematically illustrated in FIG. 29 includes a central processing unit (CPU) 1592, which may include a general purpose programmable computer, a microprocessor, a programmable logic controller, and the like. The CPU is coupled to the flow rate adjusting unit 1584 via the signal transmission line 1590 and to the semiconductor manufacturing equipment 1588 via the signal transmission line 1596. Thus, the CPU is configured to receive input from the fluid circuit flow control unit 1584. For example, the flow control unit 1584 includes a flow monitoring device in the fluid circuit, and transmits a signal indicating the flow of the fluid to the semiconductor manufacturing facility 1588 to the CPU through the signal transmission line 1590. The CPU is then coupled to the heating regulator unit 1578 via a signal transmission line 1594.

[00318] The semiconductor manufacturing facility 1588 further sends a signal indicating a change in one or more parameters of the semiconductor manufacturing facility correlated to the amount of fluid required by the facility to the CPU 1592 via the signal transmission line 1596. It is also configured to output.

[00319] Accordingly, if either or both of the flow control unit 1584 or the semiconductor manufacturing facility 1588 outputs a signal to the CPU 1592 on line 1590 or 1596 indicating that further fluid must flow through the fluid circuit to the facility, the CPU Accordingly, a signal is transmitted to the heating regulator unit 1578 on the signal transmission line 1594 and the heating jacket 1572 increases the level of heating of the container 1570, for example, by increasing the electrical input to the heating jacket. .

[00320] Since the valve of the system of FIG. 29 is a high conductivity flow control valve, the dispensing of fluid from the vessel 70 allows the semiconductor manufacturing facility to operate at low pressure conditions and maintain fluid flow at a significant rate. If necessary, it can be done in a very efficient way.

[00321] The present invention has been described with reference to specific aspects, features and exemplary embodiments of the invention, as will be readily apparent to one of ordinary skill in the art based on the disclosure herein. However, it will be appreciated that the utility of the present invention is not limited thereto, but rather extends to and encompasses numerous other variations, modifications, and alternative embodiments. . Accordingly, the invention is to be broadly understood as including all such modifications, alterations, and alternative embodiments as set forth in the claims without departing from the spirit and scope of the invention. And is intended to be interpreted.

[0030] FIG. 6 is a schematic front view showing a partial cross-section of a system for delivering reagents from solid source material, according to one embodiment of the present invention. [0031] FIG. 6 is a schematic front view showing a partial cross section of a system for delivering reagents from solid source material according to another embodiment of the present invention. [0032] FIG. 6 is a schematic diagram illustrating a configuration for depositing vapor of a solid source material on a physical adsorption medium in a storage and distribution vessel. [0033] FIG. 4 is a schematic diagram illustrating the storage and distribution vessel of FIG. 3 in a subsequent distribution mode in which adsorbed feedstock material is desorbed and utilized in a downstream fluid utilization process system. [0034] FIG. 7 is a perspective view of a source reagent article according to another embodiment of the present invention, including a core body, coated with a solid source material. [0035] FIG. 6 is a schematic illustration of a delivery system using solid source material according to yet another embodiment of the present invention. [0036] FIG. 4 is a diagram of a reagent delivery system using solid source material according to another embodiment of the present invention. [0037] FIG. 6 is a diagram of a reagent delivery system using solid source material, according to additional embodiments of the invention. [0038] FIG. 6 is a schematic perspective view of an annular reagent dispensing container according to another aspect of the present invention, adapted to allow internal positioning of a heating jacket on an outer surface along with a heating insert. [0039] Partial cross-section of a reagent delivery container according to an embodiment of the invention, comprising a series of horizontal trays, each of which is coated with a solid source material or containing a solid source material, FIG. [0040] FIG. 9 is a perspective view showing a partial cross section of a reagent delivery container according to another aspect of the present invention incorporating an internal fluid recovery manifold associated with a porous tube and / or porous ring. [0041] FIG. 4 is a diagram of a horizontal reagent delivery container illustrating solids evaporation techniques according to another aspect of the present invention. [0042] FIG. 6 is a schematic illustration of a reagent delivery system according to another embodiment of the invention comprising a buffer zone. [0043] FIG. 10 is a perspective view of a reagent delivery container inserted into a conformally shaped heating jacket, illustrating another aspect of the present invention in another embodiment. [0044] Reagent delivery container according to another aspect of the present invention showing an associated monitoring and control component comprising a recovery manifold member coupled to a porous recovery tube to release evaporated solid vapor from the container It is a perspective view which shows a partial cross section. [0045] The elongated support member is coated with a solid source material, so that the coated article is passed through the heating zone in a translational manner so that the solid source material evaporates and forms a vapor for the fluid utilization device. 1 is a schematic front sectional view. [0046] Adsorbent high thermal conductivity particles and adsorbent high thermal conductivity particles in a mixture exhibiting a surface coating of the solid raw material, wherein the mass of particles is subjected to energy to mediate evaporation of the solid raw material It is a section schematic diagram showing a part of. [0047] FIG. 6 is a schematic illustration of a conveyor system for translating particles of a solid source material through a heating zone to evaporate the solid source material and form steam for use in a steam utilization process. [0048] FIG. 6 is a schematic diagram of a fluidized bed system for generating steam from a solid source material coated on substrate particles and utilizing the resulting steam in a downstream fluid utilization facility. [0049] FIG. 6 is a schematic diagram of a steam generation system using solid source material, equipped with various monitoring and control components as accessories. [0050] FIG. 6A is a front view illustrating a partial cross-section of a solid source reagent delivery package, according to one embodiment of the present invention. [0051] FIG. 6 is a front view of a solid source reagent delivery package covered with a shrink wrap film as a safety protection and tamper-evident function. [0052] Heat flux sensor readings in units of DC, volts in temperature, as a function of elapsed time in minutes, at various locations in the source reagent supply package, according to an embodiment of the invention It is a graph of a value. [0053] FIG. 8 is a front view showing a partial cross-section of a solid source reagent delivery package according to another embodiment of the present invention. [0054] FIG. 3 is a perspective view of a highly conductive valve according to an embodiment of the invention. [0055] FIG. 26 is a top view of the highly conductive valve of FIG. [0056] FIG. 26 is a front view of the highly conductive valve of FIG. [0057] FIG. 28 is a cross-sectional front view of the highly conductive valve of FIG. 27 taken along line AA. [0058] A heating jacket is disposed for heating in response to a required amount of fluid in the semiconductor manufacturing facility, configured to communicate with the fluid circuit in a fluid flow to deliver fluid to the semiconductor manufacturing facility, 1 is a schematic diagram of a solid source reagent storage and dispensing container incorporating the highly conductive valve of the present invention.

Claims (17)

An ion implantation system,
(A) A gas configured to hold a reagent supply container that can withstand accidental overpressures of 1500 pounds per square inch or more that is contaminated during operation and requires cleaning to maintain its performance. An ion implanter including a box;
(B) a source of XeF ₂ chemical substance having a solid source reagent supply container in the gas box ,
The reagent supply container comprises an internal volume solid XeF ₂ is on, Ru is configured to the XeF ₂ vapor from said solid XeF ₂ of the reagent supply container sent for that cleaning the ion implantation apparatus together with the in the interior volume includes additional surface area structures, and is configured to be able to withstand accidental overpressure more than 1500 lbs / square inch in order to support the solid XeF _2,
The additional surface area structure within the internal volume of the reagent supply container has a metal foam having a diameter substantially equal to the inner diameter of the container, and the solid XeF ₂ is received in a hole of the metal foam. look including a solid XeF ₂ particles,
The source further comprises a valve having a valve flow coefficient C _V of at least 2 attached to the reagent supply container for delivering the XeF ₂ vapor .
Ion implantation system. The reagent supply container comprises structural components of different materials, the structural components being explosively crimped together;
The ion implantation system according to claim 1. The different materials include aluminum and steel,
The ion implantation system according to claim 2 . A fluorine chemical source for cleaning an ion implanter,
A solid source reagent supply container including an internal volume;
A metal foam for holding a solid fluorine raw material,
The metal foam, with to such a shape in contact with the interior wall of the interior volume have a diameter approximately equal to the inner diameter of the container, which the metal foam at ambient conditions by, said thermal solid fluorine raw material The solid fluorine source material includes solid XeF ₂ particles housed in the pores of the metal foam ,
Comprising a valve having a valve flow coefficient C _V of at least 2 attached to the vessel for delivering XeF ₂ vapor ;
Fluorine chemical source. The metal foam includes an aluminum foam,
The fluorine chemical substance source according to claim 4 . The metal foam includes a stacked array of disks of metal foam material therein,
The fluorine chemical substance source according to claim 4 . The valve has a valve flow coefficient in the range of 2.7 to 2.9 and has an inlet passage and an outlet passage perpendicular to each other;
The fluorine chemical substance source according to claim 4 . And a fluid circuit coupled to the reagent supply container for supplying vapor from the solid fluorine source material for cleaning to the ion implanter and connecting the reagent supply container to the ion implanter in a vapor supply relationship. Comprising
The fluorine chemical substance source according to claim 4 . The reagent supply container and the fluid circuit are configured so that the vapor does not condense in the fluid circuit.
The fluorine chemical substance source according to claim 8 . The fluid circuit includes a flow control unit selected from a flow instrumentation, a sensor, a mobile fluid drive, a mass flow controller, a pressure transducer, a surge tank, a pump, a compressor, and a flow control valve.
The fluorine chemical substance source according to claim 9 . Including a solid fluorine source material configured to deliver steam from the solid fluorine source material at or near room temperature (25 ° C.),
The fluorine chemical substance source according to claim 4 . The reagent supply container is configured to maintain a temperature in the range of 20 ° C. to 30 ° C.,
The fluorine chemical substance source according to claim 4 . The reagent supply container is formed of aluminum, and the metal foam is formed of aluminum.
The fluorine chemical substance source according to claim 4 . The container comprises a structural part including a first part made of steel and a second part made of aluminum, the first and second parts being explosively crimped together;
The fluorine chemical substance source according to claim 4 . The first part is a stainless steel flange member.
The fluorine chemical source according to claim 14 . A method of supplying xenon difluoride for cleaning an ion implanter, comprising:
Storing solid XeF ₂ particles in pores of a porous aluminum foam disposed within the enclosed internal volume of the container ;
And generating a XeF ₂ vapor from said solid XeF ₂ particles that are stored in the pores of the porous aluminum foam,
Releasing the XeF ₂ vapor from the vessel through a valve having a valve flow coefficient C _V of at least 2 ;
See containing and a washing said ion implanter by flowing the XeF ₂ vapor in the ion implantation apparatus,
The aluminum foam has a diameter approximately equal to the inner diameter of the container;
Method. The container includes an aluminum container disposed in a gas box of the ion implanter ,
The method of claim 16 .

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